Novel aerosol-generating matrix containing dill species
By using homogenized plant material formed by dill seed particles as an aerosol generation matrix, the problem of insufficient flavor and full mouthfeel in heated aerosol generation products is solved, and the effects of efficient manufacturing and compound reduction are achieved.
Patent Information
- Application Number
- CN202180044623.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Priority Date
- 2020-06-30
- Filing Date
- 2021-06-28
- Publication Date
- 2025-10-03
- Estimated Expiration
- 2041-06-28
AI Technical Summary
Existing heated aerosol-generating articles have difficulty in providing an aerosol experience with similar flavor and mouthfeel to conventional combustible cigarettes, while also containing certain undesirable aerosol compounds and being difficult to manufacture efficiently in existing equipment.
Homogenized plant material formed by dill seed particles is used as an aerosol generating matrix, an aerosol former and a binder are added to ensure that the matrix contains at least 100 micrograms of carvone and 2 micrograms of limonene, and the matrix is made into sheets or strips through a casting or extrusion process, and then dried to form an aerosol generating matrix.
The invention provides an improved flavor and mouthfeel aerosol experience, significantly reduces certain undesirable aerosol compounds, such as polycyclic aromatic hydrocarbons and phenolic compounds, while maintaining nicotine levels, and can be efficiently manufactured in existing equipment.
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Figure CN115843221B_ABST
Abstract
Description
[0001] The present invention relates to an aerosol-generating substrate comprising homogenized plant material formed from dill seed particles and an aerosol-generating article incorporating such an aerosol-generating substrate. The present invention also relates to an aerosol derived from an aerosol-generating substrate comprising dill seed particles.
[0002] Aerosol-generating articles are known in the art, in which an aerosol-generating substrate (such as a tobacco-containing substrate) is heated rather than combusted. Typically, in such articles, an aerosol is generated by transferring heat from a heat source to a physically separate aerosol-generating substrate or material, which may be positioned in contact with, within, around, or downstream of the heat source. During use of the aerosol-generating article, volatile compounds are released from the substrate by heat transfer from the heat source and are entrained in air drawn through the article. When the released compounds cool, they condense to form an aerosol.
[0003] Some aerosol-generating articles contain flavoring agents that are delivered to the consumer during use of the article to provide the consumer with a different sensory experience, for example, to enhance the flavor of the aerosol. Flavoring agents can be used to deliver taste (flavor), smell (smell), or both taste and smell to a user inhaling the aerosol. It is known to provide heated aerosol-generating articles that contain flavoring agents.
[0004] It is also known to provide flavorings in conventional combustible cigarettes, which are smoked by lighting the end of the cigarette opposite the mouthpiece, causing the tobacco rod to combust and generate inhalable smoke. One or more flavorings are typically mixed with the tobacco in the tobacco rod to provide additional flavor to the mainstream smoke as the tobacco combusts. Such flavorings can be provided, for example, in the form of essential oils.
[0005] Aerosols from conventional cigarettes, which contain a large number of components that interact with receptors located in the mouth, provide a "full mouthfeel," that is, a relatively full mouthfeel. As used herein, "mouthfeel" refers to the physical sensation in the mouth caused by food, beverages, or aerosols, and is distinct from taste. It is a fundamental sensory attribute that, along with taste and odor, determines the overall flavor of a food or aerosol.
[0006] There are difficulties in reproducing the consumer experience provided by conventional combustible cigarettes using aerosol-generating articles in which the aerosol-generating substrate is heated rather than combusted. This is due in part to the lower temperatures reached during heating of such aerosol-generating articles, which results in a different distribution of volatile compounds released.
[0007] It would be desirable to provide a novel aerosol-generating substrate for heated aerosol-generating articles that provides an aerosol with improved flavor and full mouthfeel. It would be particularly desirable if such an aerosol-generating substrate could provide an aerosol with a sensory experience comparable to that provided by conventional combustible cigarettes. It would also be particularly desirable if such an aerosol-generating substrate could provide reduced levels of undesirable aerosol compounds compared to existing aerosol-generating substrates (e.g., those containing only tobacco).
[0008] It would also be desirable to provide an aerosol-generating substrate that can be easily incorporated into an aerosol-generating article and that can be manufactured using existing high-speed methods and equipment.
[0009] The present disclosure relates to an aerosol-generating article comprising an aerosol-generating substrate formed from a homogenized plant material containing dill seed particles, referred to herein as "homogenized dill seed material." The homogenized dill seed material may contain dill seed particles. The homogenized dill seed material may also contain an aerosol-forming agent. The homogenized dill seed material may also contain a binder. The aerosol-generating substrate may also contain at least about 100 micrograms of carvone per gram of substrate on a dry weight basis. The aerosol-generating substrate may also contain at least about 2 micrograms of limonene per gram of substrate on a dry weight basis. The amount of carvone per gram of substrate may not exceed about 50 times the amount of limonene per gram of substrate.
[0010] According to the present invention, an aerosol-generating article is provided that includes an aerosol-generating substrate formed from a homogenized dill seed material comprising dill seed particles. According to the present invention, the homogenized plant material comprises: dill seed particles; an aerosol-forming agent; and a binder. The aerosol-generating substrate further comprises at least about 100 micrograms of carvone per gram of substrate on a dry weight basis; and at least about 2 micrograms of limonene per gram of substrate on a dry weight basis. The amount of carvone per gram of substrate is no more than about 50 times the amount of limonene per gram of substrate.
[0011] Preferably, when an aerosol-generating substrate of an aerosol-generating article according to the present invention is heated according to Test Method A as described below, an aerosol is generated comprising: at least about 20 micrograms of carvone per gram of substrate on a dry weight basis; and at least about 2 micrograms of limonene per gram of substrate on a dry weight basis, wherein the amount of carvone per gram of substrate is no more than about 10 times the amount of limonene per gram of substrate.
[0012] Preferably, the aerosol generated by the aerosol-generating substrate may comprise an aerosol amount of at least about 0.5 μg of carvone per puff when the aerosol-generating substrate is heated according to Test Method A. The aerosol generated by the aerosol-generating substrate may comprise an aerosol amount of at least about 0.05 μg of limonene per puff when the aerosol-generating substrate is heated according to Test Method A. The amount of carvone per puff of the aerosol is preferably no more than about 10 times the amount of limonene per puff of the aerosol. As generated by a smoking machine, the aerosol has a volume of 55 ml per puff.
[0013] According to the present invention, an aerosol-generating article is provided that includes an aerosol-generating substrate formed from a homogenized dill seed material comprising dill seed particles. The aerosol-generating substrate comprises at least about 100 micrograms of carvone per gram of substrate on a dry weight basis; and at least about 2 micrograms of limonene per gram of substrate on a dry weight basis. The amount of carvone per gram of substrate is no more than about 50 times the amount of limonene per gram of substrate.
[0014] The present disclosure also relates to an aerosol-generating substrate formed from homogenized plant material containing dill seed particles, referred to herein as "homogenized dill seed material." The homogenized dill seed material may further comprise an aerosol-forming agent. The homogenized dill seed material may further comprise a binder. The aerosol-generating substrate may comprise at least about 100 micrograms of carvone per gram of substrate on a dry weight basis. The aerosol-generating substrate may comprise at least about 2 micrograms of limonene per gram of substrate on a dry weight basis. The amount of carvone per gram of substrate may be no more than about 50 times the amount of limonene per gram of substrate.
[0015] According to the present invention, there is also provided an aerosol-generating substrate formed from a homogenized dill seed material, wherein the homogenized dill seed material comprises dill seed particles, an aerosol-forming agent, and a binder. The aerosol-generating substrate further comprises at least 100 micrograms of carvone per gram of substrate on a dry weight basis; and at least 2 micrograms of limonene per gram of substrate on a dry weight basis, wherein the amount of carvone per gram of substrate is no more than about 50 times the amount of limonene per gram of substrate.
[0016] The present disclosure further relates to an aerosol generated upon heating an aerosol-generating substrate. The aerosol may contain carvone in an amount of at least about 0.5 micrograms per puff of the aerosol. The aerosol may contain limonene in an amount of at least about 0.05 micrograms per puff of the aerosol. The amount of carvone per gram of substrate in the aerosol may not exceed about 10 times the amount of limonene per gram of substrate in the aerosol. As generated by a smoking machine, the aerosol has a volume of 55 milliliters per puff.
[0017] According to the present invention, there is also provided an aerosol generated upon heating an aerosol-generating substrate, the aerosol comprising: carvone in an amount of at least about 0.5 micrograms per puff of the aerosol; and limonene in an amount of at least about 0.05 micrograms per puff of the aerosol, wherein the amount of carvone per gram of substrate is no more than about 10 times the amount of limonene per gram of substrate in the aerosol and wherein the aerosol has a volume of 55 milliliters per puff as generated by a smoking machine.
[0018] The present invention also provides a method for making an aerosol-generating substrate, comprising: forming a slurry comprising dill seed particles, water, an aerosol-forming agent, a binder, and optionally tobacco particles; casting or extruding the slurry into a sheet or strip form; and drying the sheet or strip, preferably at a temperature between 80 and 160 degrees Celsius. In the case of forming an aerosol-generating substrate sheet, the sheet may optionally be cut into strips or gathered to form strips. Prior to the gathering step, the sheet may optionally be crimped.
[0019] Unless otherwise stated, any reference below to aerosol-generating substrates and aerosols of the present invention should be taken to apply to all aspects of the present invention.
[0020] As used herein, the term "aerosol-generating article" refers to an article for generating an aerosol, wherein the article comprises an aerosol-generating substrate that is suitable and intended to be heated or combusted so as to release volatile compounds that can form an aerosol. A conventional cigarette will be ignited when a user applies a flame to one end of the cigarette and draws air through the other end. The localized heat provided by the flame and the oxygen in the air drawn through the cigarette causes the end of the cigarette to ignite, and the resulting combustion generates inhalable smoke. In contrast, in a "heated aerosol-generating article", the aerosol is generated by heating the aerosol-generating substrate rather than by burning the aerosol-generating substrate. Known heated aerosol-generating articles include, for example, electrically heated aerosol-generating articles and aerosol-generating articles in which the aerosol is generated by heat transfer from a combustible fuel element or heat source to a physically separate aerosol-generating substrate.
[0021] Also known are aerosol-generating articles suitable for use in an aerosol-generating system that supplies an aerosol-forming agent to the aerosol-generating article. In such systems, the aerosol-generating substrate in the aerosol-generating article contains significantly less aerosol-forming agent than an aerosol-generating substrate that carries and provides substantially all of the aerosol-forming agent used to form the aerosol during operation.
[0022] As used herein, the term "aerosol-generating substrate" refers to a substrate that is capable of generating volatile compounds upon heating, which can form an aerosol. The aerosol generated by the aerosol-generating substrate may be visible or invisible to the human eye and may contain vapor (e.g., fine particulate matter in a gaseous state that is typically liquid or solid at room temperature) as well as droplets of gas and condensed vapor.
[0023] As used herein, the term "homogenized plant material" encompasses any plant material formed by agglomeration of plant particles. For example, a sheet or web of homogenized plant material for use in the aerosol-generating substrate of the present invention can be formed by agglomerating particles of plant material obtained by comminuting, grinding, or crushing dill seed plant material and, optionally, tobacco material such as tobacco leaf flakes and stems. The homogenized plant material can be produced by casting, extrusion, papermaking, or any other suitable process known in the art.
[0024] As used herein, the term "homogenized dill seed material" refers to homogenized plant material comprising dill seed particles, optionally in combination with tobacco particles. The term "homogenized tobacco material" refers to homogenized plant material comprising tobacco particles but no dill seed particles, which is therefore not according to the present invention.
[0025] As used herein, the term "dill seed granules" encompass granules derived from the seeds of the dill plant (Anethum graveolens). Dill is an annual herb of the genus Dill in the apiaceae family, Apiaceae, and is widely grown in Europe and Asia. Dill leaves and seeds are commonly used to season foods.
[0026] In contrast, dill oil is a distillate extracted from the leaves, stems, and seeds of the plant, while carvone and limonene are compounds derived from dill seeds.
[0027] The present invention provides an aerosol-generating article incorporating an aerosol-generating substrate formed from a homogenized plant material containing dill seed particles, referred to herein as homogenized dill seed material. The present invention also provides an aerosol derived from such an aerosol-generating substrate. The inventors have discovered that by incorporating dill seed particles into the aerosol-generating substrate, an aerosol can be advantageously produced that provides a novel sensory experience. Such an aerosol provides a unique flavor and can provide an increased level of mouthfullness.
[0028] Furthermore, the inventors have discovered that aerosols with improved dill seed aroma and flavor can be advantageously produced compared to aerosols produced by adding dill seed additives, such as dill seed oil. Dill oil (CAS Reg. No. 8006-75-5) is obtained by steam distillation of the dill plant, primarily dill seeds. It has a different flavoring composition than dill seed particles, likely due to the distillation process selectively removing or retaining certain flavorings. Carvone is one of the main components of dill oil. Limonene is also present in dill oil, but at significantly lower levels than limonene.
[0029] Furthermore, in certain aerosol-generating substrates provided herein, dill seed particles can be incorporated at sufficient levels to provide a desired dill seed flavor while maintaining sufficient tobacco material to provide a desired nicotine level to the consumer.
[0030] Furthermore, it has been surprisingly discovered that the inclusion of dill seed particles in the aerosol-generating substrate provides a significant reduction in certain undesirable aerosol compounds compared to an aerosol generated from an aerosol-generating substrate comprising 100% tobacco particles without dill seed particles. In particular, as shown below, it has been surprisingly discovered that the inclusion of dill seed particles in the aerosol-generating substrate provides a significant reduction in certain polycyclic aromatic hydrocarbons (PAHs) and phenolic compounds compared to an aerosol generated from an aerosol-generating substrate comprising 100% tobacco particles without dill seed particles. Furthermore, this reduction has been found to be greater than would be expected proportionally due to the reduction in tobacco particles.
[0031] The presence of dill seeds in homogenized plant material (e.g., cast leaves) can be positively identified by DNA barcoding. Methods for DNA barcoding based on the nuclear genes ITS2, rbcL, and matK system and the plastidial gene spacer trnH-psbA are well known in the art and can be used (Chen S, Yao H, Han J, Liu C, Song J, et al. (2010) Validation of the ITS2 Region as a Novel DNA Barcode for Identifying Medicinal Plant Species. PLoS ONE 5(1):e8613; Hollingsworth PM, Graham SW, Little DP (2011) Choosing and Using a Plant DNA Barcode. PLoS ONE 6(5):e19254).
[0032] The inventors have conducted a complex analysis and characterization of aerosols generated by an aerosol-generating matrix of the present invention that has been introduced with dill seed particles and a mixture of dill seed particles and tobacco particles, and compared these aerosols with those generated by an existing aerosol-generating matrix formed by a tobacco material that does not contain dill seed particles. Based on this, the inventors have been able to identify a group of "characteristic compounds," which are compounds that are present in the aerosol and derive from the dill seed particles. Therefore, the detection of these characteristic compounds in an aerosol within a specific weight ratio can be used to identify an aerosol that derives from an aerosol-generating matrix that contains dill seed particles. These characteristic compounds are clearly absent or only present in a very low amount in an aerosol generated by the tobacco material. In addition, the ratio of the characteristic compounds in the aerosol and the ratio of the characteristic compounds to each other clearly indicate that dill seed plant material rather than dill oil has been used. Similarly, the presence of these characteristic compounds in a specific ratio in the aerosol-generating matrix indicates that the matrix contains dill seed particles.
[0033] Specifically, the defined levels and ratios of characteristic compounds within the matrix and aerosol are specific to the dill seed particles present within the homogenized dill seed material. The level of each characteristic compound depends on how the dill seed particles are processed during production of the homogenized dill seed material. The level also depends on the composition of the homogenized dill seed material and, in particular, will be influenced by the levels of other components within the homogenized dill seed material. The level of a characteristic compound within the homogenized dill seed material will differ from the level of the same compound within the starting dill seed material. It will also differ from the level of a characteristic compound within a material containing dill seed particles but not according to the present invention as defined herein.
[0034] To characterize the aerosols, the inventors utilized complementary non-targeted differential screening (NTDS) using liquid chromatography coupled to high-resolution accurate mass spectrometry (LC-HRAM-MS) in parallel with two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GCxGC-TOFMS).
[0035] Non-targeted screening (NTS) is a key approach to characterize the chemical composition of complex matrices by elucidating the structure of unknown compounds by matching the signatures of detected compounds to a spectral database (suspect screening analysis [SSA]) or, if there is no prior knowledge of a match, by matching information obtained using, for example, first-order fragmentation (MS / MS) to in silico predicted fragments from a compound database (non-targeted analysis [NTA]). It enables the simultaneous measurement of a large number of small molecules from a sample using an unbiased approach and the semi-quantification of these small molecules.
[0036] If, as described above, the focus is on comparing two or more aerosol samples, evaluating any significant differences in chemical composition between the samples in an unsupervised manner, or if group-related foreknowledge between sample groups is available, non-targeted differential screening (NTDS) can be performed. A complementary differential screening approach has been applied, using liquid chromatography coupled to high-resolution accurate mass spectrometry (LC-HRAM-MS) in parallel with two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GCxGC-TOFMS) in order to ensure comprehensive analytical coverage for identifying the most relevant differences in aerosol composition between aerosols derived from a preparation comprising 100% by weight of dill seeds as the particulate plant material and those derived from a preparation comprising 100% by weight of tobacco as the particulate plant material.
[0037] Aerosols were generated and collected using the apparatus and methods described in detail below.
[0038] Using Thermo QExactive TMHigh-resolution mass spectrometers were used for LC-HRAM-MS analysis in full scan mode and data-dependent mode. Three different methods were used to cover a wide range of substances with different ionization properties and compound classes. Samples were analyzed using RP chromatography using heated electrospray ionization (HESI) in both positive and negative modes and atmospheric pressure chemical ionization (APCI) in positive mode. These methods are described in: Arndt, D. et al., "Indepth characterization of chemical differences between heat-not-burn tobacco products and cigarettes using LC-HRAM-MS-based non-targeted differential screening" (DOI: 10.13140 / RG.2.2.11752.16643); Wachsmuth, C. et al., "Comprehensivechemical character of complex matrices through integration of multiple analyticalisation and modes" databases for LC-HRAM-MS-based non-targeted screening" (DOI: 10.13140 / RG.2.2.12701.61927); and "Buchholz, C. et al., "Increasing confidence for compound identification by fragmentation database and in silicofragmentation comparison with LC-HRAM-MS-based non-targeted screening of complex matrices”(DOI:10.13140 / RG.2.2.17944.49927), both from the 66th ASMS Conference on Mass Spectrometry and Allied Topics, San Diego, USA (2018).These methods are also described in: Arndt, D. et al., "A complex matrix characterization approach, applied to cigarette smoke, that integrates multiple analytical methods and compound identification strategies for non-targeted liquid chromatography with high-resolution mass spectrometry" (DOI: 10.1002 / rcm.8571).
[0039] The LECO Pegasus 4D was used with an automatic liquid sampler (7683B). TM GCxGC-TOFMS analysis was performed using an Agilent GC 6890A or 7890A instrument coupled to a mass spectrometer with a thermostat, using three different methods for non-polar, polar, and highly volatile compounds in the aerosol. These methods are described in: Almstetter et al., “Non-targeted screening using GC×GC-TOFMS for in-depth chemical characterization of aerosol from a heat-not-burn tobacco product” (DOI: 10.13140 / RG.2.2.36010.31688 / 1); and Almstetter et al., “Non-targeted differential screening of complex matrices using GC×GC-TOFMS for comprehensive characterization of the chemical composition and determination of significant differences” (DOI: 10.13140 / RG.2.2.32692.55680), from the 66th and 64th ASMS Conferences on Mass Spectrometry and Allied Topics, San Diego, USA, respectively.
[0040] The results of the analytical methods provide information on the main compounds responsible for the differences in the aerosols produced by these products. Non-targeted differential screening using the analytical platforms LC-HRAM-MS and GCxGC-TOFMS focused on compounds that were present in greater amounts in the aerosols of samples of the aerosol-forming matrix according to the present invention, comprising 100% dill seed particles, relative to a comparative sample of an aerosol-forming matrix comprising 100% tobacco particles. The NTDS method is described in the aforementioned literature.
[0041] Based on this information, the inventors were able to identify specific compounds within the aerosol that can be considered "signature compounds" originating from the dill seed particles in the matrix. Signature compounds derived from dill seeds include, but are not limited to: limonene (1-methyl-4-(prop-1-en-2-yl)cyclohex-1-ene, chemical formula: C 10 H 16 , Chemical Abstracts Service Registry No. 138-86-3); and carvone (2-methyl-5-(prop-1-en-2-yl)cyclohex-2-en-1-one, chemical formula: C 10 H 20 O, Chemical Abstracts Service Registry No. 99-49-0).
[0042] For the purposes of the present invention, a sample of an aerosol-generating substrate can be subjected to targeted screening to identify the presence and amount of each characteristic compound in the substrate. This targeted screening method is described below. As described, characteristic compounds can be detected and measured in an aerosol-generating substrate and an aerosol derived from the aerosol-generating substrate.
[0043] As defined above, the aerosol-generating article of the present invention comprises an aerosol-generating substrate formed from a homogenized plant material comprising dill seed particles. By virtue of comprising the dill seed particles, the aerosol-generating substrate comprises a proportion of the "characteristic compounds" of dill seed, as described above. In particular, the aerosol-generating substrate preferably comprises, on a dry weight basis, at least 100 micrograms of carvone per gram of substrate and at least 2 micrograms of limonene per gram of substrate.
[0044] For the purposes of the present invention, the amount of carvone should be considered as the total combined amount of the carvone stereoisomers: L-carvone and D-carvone. Similarly, the amount of limonene should be considered as the total combined amount of the limonene stereoisomers: L-limonene and D-limonene.
[0045] By defining the aerosol-generating matrix relative to the desired level of characteristic compounds, consistency between products can be ensured despite potential differences in the levels of characteristic compounds in the raw materials. This advantageously enables more effective control of product quality.
[0046] Preferably, the aerosol-forming substrate comprises at least about 250 μg of carvone / g of substrate, more preferably at least about 500 μg of carvone / g of substrate, on a dry weight basis. Alternatively or additionally, the aerosol-forming substrate preferably comprises no more than about 4500 μg of carvone / g of substrate, more preferably no more than about 4000 μg of carvone / g of substrate, more preferably no more than about 3000 μg of carvone / g of substrate, on a dry weight basis.
[0047] For example, the aerosol-generating substrate may comprise, on a dry weight basis, from about 100 micrograms to about 4500 micrograms of carvone per gram of substrate, or from about 250 micrograms to about 4000 micrograms of carvone per gram of substrate, or from about 500 micrograms to about 3000 micrograms of carvone per gram of substrate.
[0048] In certain preferred embodiments, the aerosol-forming substrate may comprise from about 100 μg to about 1500 μg of carvone per gram of aerosol-forming substrate, more preferably from about 250 μg to about 1000 μg of carvone per gram of aerosol-forming substrate. For example, the level of carvone may be within these ranges for the first preferred embodiment of the invention, wherein the aerosol-forming substrate comprises from 2.5 wt% to 25 wt% dill seed particles on a dry weight basis, as described below.
[0049] Preferably, the aerosol-forming substrate comprises at least about 10 μg limonene / gram substrate, more preferably at least about 25 μg limonene / gram substrate on a dry weight basis. Alternatively or additionally, the aerosol-forming substrate preferably comprises no more than about 200 μg limonene / gram substrate, more preferably no more than about 150 μg limonene / gram substrate, and even more preferably no more than about 100 μg limonene / gram substrate on a dry weight basis.
[0050] For example, the aerosol-forming substrate may comprise, on a dry weight basis, from about 2 micrograms to about 200 micrograms of limonene per gram of substrate, or from about 10 micrograms to about 150 micrograms of limonene per gram of substrate, or from about 25 micrograms to about 100 micrograms of limonene per gram of substrate.
[0051] In certain particularly preferred embodiments, the aerosol-forming substrate may comprise from about 2 μg to about 50 μg of limonene per gram of aerosol-forming substrate, more preferably from about 10 μg to about 40 μg of limonene per gram of aerosol-forming substrate. For example, the limonene levels may be within these ranges for the first preferred embodiment of the present invention, wherein the aerosol-forming substrate comprises from 2.5% to 25% by weight, on a dry weight basis, of dill seed particles, as described below.
[0052] As defined above, the ratio of the characteristic compounds in the aerosol-forming substrate is such that the amount of carvone per gram of substrate is no more than about 50 times the amount of limonene per gram of substrate, more preferably no more than about 40 times the amount of limonene per gram of substrate, and more preferably no more than about 35 times the amount of limonene per gram of substrate. Thus, the ratio of carvone to limonene in the aerosol-forming substrate is significantly lower than the ratio of carvone to limonene in dill oil, as the relative proportion of carvone is much higher in the oil compared to dill seed particles.
[0053] Thus, the carvone to limonene ratio is characteristic of the inclusion of dill seed particles in the aerosol-forming matrix.
[0054] The present invention also provides an aerosol-generating article comprising an aerosol-generating substrate formed from homogenised plant material comprising dill seed particles, as defined above, wherein upon heating the aerosol-generating substrate an aerosol comprising a "signature compound" of dill seed is generated.
[0055] For the purposes of the present invention, the aerosol-generating substrate is heated according to "Test Method A". In Test Method A, an aerosol-generating article incorporating an aerosol-generating substrate is heated in a Tobacco Heating System 2.2 holder (THS2.2 holder) under the Health Canada machine smoking protocol. For the purposes of performing Test Method A, the aerosol-generating substrate is provided in an aerosol-generating article that is compatible with the THS2.2 holder.
[0056] The Tobacco Heating System 2.2 holder (THS2.2 holder) corresponds to the commercially available IQOS device (Philip Morris Products SA (Switzerland)), as described in Smith et al., 2016, Regul. Toxicol. Pharmacol. 81 (S2) S82-S92. Aerosol-generating articles for use in conjunction with the IQOS device are also commercially available.
[0057] The Health Canada smoking protocol is a well-defined and accepted smoking protocol as defined in Health Canada 2000 - Tobacco Products Information Regulations SOR / 2000-273, Schedule 2, published by the Ministry of Justice Canada. The test method is described in ISO / TR 19478-1:2014. In the Health Canada smoking test, 12 aerosol puffs are collected from a sample aerosol-generating substrate with a puff volume of 55 mm, a puff duration of 2 seconds, a puff interval of 30 seconds, and all ventilation, if present, is blocked.
[0058] Therefore, in the context of the present invention, the expression "when the aerosol-generating substrate is heated according to Test Method A" means when the aerosol-generating substrate is heated in a THS2.2 holder under the Health Canada machine smoking protocol as defined in Health Canada 2000 - Tobacco Product Information Regulations SOR / 2000-273, Plan 2, published by the Ministry of Justice Canada, which test method is described in ISO / TR 19478-1:2014.
[0059] With regard to the purpose of analysis, according to analytical method to be used, the aerosol generated by matrix generation by heating aerosol is captured using suitable equipment. In the suitable method for the sample analyzed by LC-HRAM-MS, regulated 44mm Cambridge glass fiber filter pad (according to ISO 3308) and filter paper clip (according to ISO 4387 and ISO 3308) are used to capture the particle phase. Two continuous micro-dust analyzers (20mL) are used to collect the remaining gas phase from the filter pad downstream, and the micro-dust analyzer comprises methanol and internal standard (ISTD) solution (10mL) separately, uses dry ice-isopropanol mixture to maintain-60 degrees Celsius. Then the particle phase and gas phase of capture are merged again, and use the methanol from micro-dust analyzer to extract by oscillation sample, vortex 5 minutes and centrifugal (4500g, 5 minutes, 10 ℃). Gained extract is diluted with methanol, and mixed in Eppendorf ThermoMixer (5 ℃, 2000rpm). Test samples from the extract were analyzed by LC-HRAM-MS in a combined full scan mode and data dependent fragmentation mode to identify characteristic compounds.For the purposes of the present invention, LC-HRAM-MS analysis is suitable for the identification and quantification of carvone.
[0060] Samples for GCxGC-TOFMS analysis can be generated in a similar manner, but for GCxGC-TOFMS analysis, different solvents are suitable for extracting and analyzing polar compounds, non-polar compounds, and volatile compounds separated from the whole aerosol.
[0061] For non-polar and polar compounds, regulated 44mm Cambridge glass fiber filter pad (according to ISO3308) and filter paper clip (according to ISO 4387 and ISO 3308) are used, and then two micro dust testers connected in series and sealed are used to collect whole aerosols. Each micro dust tester (20mL) comprises 10mL dichloromethane / methanol (80:20v / v), which comprises internal standard (ISTD) and retention index marker (RIM) compound. Micro dust tester is maintained at -80 ℃ using dry ice-isopropanol mixture. In order to analyze non-polar compounds, the content of micro dust tester is used to extract the particle phase of whole aerosol from glass fiber filter pad. Water is added in aliquots (10mL) of the obtained extract, and shaken and centrifuged as described above. The dichloromethane layer is separated, dried with sodium sulfate, and analyzed in full scan mode by GCxGC-TOFMS. In order to analyze polar compounds, the remaining water layer prepared from the above-mentioned non-polar sample is used. ISTD and RIM compounds were added to the aqueous layer and then directly analyzed by GCxGC-TOFMS in full scan mode.
[0062] For volatile compounds, the whole aerosol was collected using two sealed micro-dust analyzers (20 mL) connected in series, each filled with 10 mL of N,N-dimethylformamide (DMF) containing ISTD and RIM compounds. The micro-dust analyzers were maintained at -50°C to -60°C using a dry ice-isopropanol mixture. After collection, the contents of the two micro-dust analyzers were combined and analyzed by GCxGC-TOFMS in full-scan mode.
[0063] For the purposes of the present invention, GCxGC-TOFMS analysis is suitable for the identification and quantification of carvone and limonene.
[0064] The aerosol generated upon heating an aerosol-forming substrate of the invention according to Test Method A is preferably characterised by the amounts and ratios of the characteristic compounds carvone and limonene as defined above.
[0065] Preferably, in an aerosol-generating article comprising an aerosol-generating substrate as described above, upon heating the aerosol-generating substrate according to Test Method A, an aerosol is generated comprising: at least about 20 micrograms of carvone per gram of substrate on a dry weight basis; and at least about 2 micrograms of limonene per gram of substrate on a dry weight basis. Preferably, the amount of carvone in the aerosol per gram of substrate is no more than about 10 times the amount of limonene in the aerosol per gram of substrate.
[0066] The ranges define the amount of each characteristic compound in the aerosol generated per gram of aerosol-generating substrate (also referred to herein as "substrate"). This is equal to the total amount of the characteristic compound measured in the aerosol collected during Test Method A divided by the dry weight of the aerosol-generating substrate before heating.
[0067] Preferably, the aerosol generated comprises at least about 100 micrograms of carvone per gram of substrate on a dry weight basis when the aerosol-generating substrate is heated according to Test Method A. More preferably, the aerosol generated from the aerosol-generating substrate according to the present invention comprises at least about 200 micrograms of carvone per gram of substrate on a dry weight basis.
[0068] Alternatively or additionally, the aerosol generated from the aerosol-generating substrate preferably comprises at most about 1500 micrograms of carvone per gram of substrate on a dry weight basis. More preferably, the aerosol generated from the aerosol-generating substrate comprises at most about 1200 micrograms of carvone per gram of substrate on a dry weight basis. Even more preferably, the aerosol generated from the aerosol-generating substrate comprises at most about 1000 micrograms of carvone per gram of substrate on a dry weight basis.
[0069] In certain embodiments of the invention, the aerosol generated from the aerosol-generating substrate may comprise up to 500 micrograms of carvone per gram of substrate, more preferably up to 300 micrograms of carvone per gram of substrate, on a dry weight basis. For example, the level of carvone may be within these ranges for the first preferred embodiment of the invention, wherein the aerosol-generating substrate comprises from 2.5% to 25% by weight of dill seed particles on a dry weight basis, as described below.
[0070] When the aerosol-forming substrate is heated according to Test Method A, the generated aerosol preferably comprises at least about 20 micrograms of limonene per gram of substrate on a dry weight basis. More preferably, the aerosol generated from an aerosol-forming substrate according to the present invention comprises at least about 50 micrograms of limonene per gram of substrate on a dry weight basis.
[0071] Alternatively or additionally, the aerosol generated from the aerosol-generating substrate preferably comprises at most about 300 micrograms of limonene per gram of substrate on a dry weight basis. More preferably, the aerosol generated from the aerosol-generating substrate comprises at most about 250 micrograms of limonene per gram of substrate on a dry weight basis. Even more preferably, the aerosol generated from the aerosol-generating substrate comprises at most about 200 micrograms of limonene per gram of substrate on a dry weight basis.
[0072] In certain embodiments of the invention, the aerosol generated from the aerosol-generating substrate may comprise up to 100 micrograms of limonene per gram of substrate, more preferably up to 75 micrograms of limonene per gram of substrate, on a dry weight basis. For example, the level of carvone may be within these ranges for the first preferred embodiment of the invention, wherein the aerosol-generating substrate comprises from 2.5% to 25% by weight of dill seed particles on a dry weight basis, as described below.
[0073] Preferably, the aerosol generated from an aerosol-generating substrate according to the present invention during Test Method A also comprises at least about 0.1 micrograms of nicotine per gram of substrate, more preferably at least about 1 microgram of nicotine per gram of substrate, and more preferably at least about 2 micrograms of nicotine per gram of substrate. Preferably, the aerosol comprises at most about 10 micrograms of nicotine per gram of substrate, more preferably at most about 7.5 micrograms of nicotine per gram of substrate, and more preferably at most about 4 micrograms of nicotine per gram of substrate. For example, the aerosol may comprise from about 0.1 micrograms to about 10 micrograms of nicotine per gram of substrate, or from about 1 microgram to about 7.5 micrograms of nicotine per gram of substrate, or from about 2 micrograms to about 4 micrograms of nicotine per gram of substrate. In some embodiments of the present invention, the aerosol may contain zero micrograms of nicotine.
[0074] Various methods known in the art can be applied to measure the amount of nicotine in the aerosol.
[0075] Carbon monoxide may also be present in the aerosol generated by an aerosol-generating substrate according to the present invention during Test Method A and may be measured and used to further characterize the aerosol. Nitrogen oxides, such as nitric oxide and nitrogen dioxide, may also be present in the aerosol and may be measured and used to further characterize the aerosol.
[0076] According to the present invention, the aerosol generated by the aerosol-generating substrate during Test Method A preferably has an amount of carvone per gram of substrate that is preferably no more than 10 times the amount of limonene per gram of substrate. Thus, the ratio of carvone to limonene is no more than 10:1. More preferably, the amount of carvone per gram of substrate in the aerosol generated by the aerosol-generating substrate during Test Method A does not exceed 8 times the amount of limonene, such that the ratio of carvone to limonene is no more than 8:1.
[0077] This defined ratio of carvone to limonene characterizes an aerosol derived from dill seed particles. In contrast, the ratio of carvone to limonene in an aerosol generated from dill oil will be significantly different due to the much higher relative proportion of carvone present in the oil relative to the dill seed particles.
[0078] The aerosol generated from the aerosol-generating substrate according to the present invention during Test Method A may also contain at least about 5 mg of aerosol-forming agent per gram of aerosol-generating substrate, or at least about 10 mg of aerosol-forming agent per gram of substrate, or at least about 15 mg of aerosol-forming agent per gram of substrate. Alternatively or additionally, the aerosol may contain up to about 30 mg of aerosol-forming agent per gram of substrate, or up to about 25 mg of aerosol-forming agent per gram of substrate, or up to about 20 mg of aerosol-forming agent per gram of substrate. For example, the aerosol may contain from about 5 mg to about 30 mg of aerosol-forming agent per gram of substrate, or from about 10 mg to about 25 mg of aerosol-forming agent per gram of substrate, or from about 15 mg to about 20 mg of aerosol-forming agent per gram of substrate. In alternative embodiments, the aerosol may contain less than 5 mg of aerosol-forming agent per gram of substrate. This may be appropriate, for example, if the aerosol-forming agent is provided separately within the aerosol-generating article or aerosol-generating device.
[0079] Suitable aerosol formers for use in the present invention are described below.
[0080] Various methods known in the art can be applied to measure the amount of aerosol-forming agent in an aerosol.
[0081] As described above, the presence of characteristic compounds in defined amounts and ratios in the aerosol is indicative of the inclusion of dill seed particles in the homogenised plant material forming the aerosol-generating matrix.
[0082] Preferably, the aerosol-generating substrate of an aerosol-generating article according to the present invention comprises a homogenized dill seed material comprising at least about 2.5% by weight of dill seed particles on a dry weight basis. Preferably, the homogenized dill seed material comprises at least about 3% by weight of dill seed particles, more preferably at least about 4% by weight of dill seed particles, more preferably at least about 5% by weight of dill seed particles, more preferably at least about 6% by weight of dill seed particles, more preferably at least about 7% by weight of dill seed particles, more preferably at least about 8% by weight of dill seed particles, more preferably at least about 9% by weight of dill seed particles, more preferably at least about 10% by weight of dill seed particles, on a dry weight basis.
[0083] The homogenized dill seed material may comprise up to about 100% by weight of dill seed particles on a dry weight basis. Preferably, the homogenized plant material comprises up to about 90% by weight of dill seed particles on a dry weight basis, more preferably up to about 80% by weight of dill seed particles, more preferably up to about 70% by weight of dill seed particles, more preferably up to about 60% by weight of dill seed particles, and more preferably up to about 50% by weight of dill seed particles.
[0084] For example, the homogenized dill seed material can comprise, on a dry weight basis, from about 2.5% to about 100% by weight dill seed particles, or from about 5% to about 90% by weight dill seed particles, or from about 10% to about 80% by weight dill seed particles, or from about 15% to about 70% by weight dill seed particles, or from about 20% to about 60% by weight dill seed particles, or from about 30% to about 50% by weight dill seed particles.
[0085] In certain particularly preferred embodiments of the present invention, the homogenized dill seed material comprises from about 15% to about 20% by weight dill seed particles on a dry weight basis.
[0086] The amount by weight of dill seed particles that can be incorporated into a homogenized dill seed material while providing usable material for an aerosol-generating article can depend to some extent on the composition of the homogenized dill seed material. For example, the maximum amount of dill seed particles that can be incorporated into a homogenized dill seed material can depend on the properties of the binder, as described below.
[0087] According to a first preferred embodiment of the present invention, the homogenized dill seed material comprises at most about 25 wt% dill seed particles, preferably at most about 24 wt% dill seed particles, more preferably at most about 23 wt% dill seed particles, more preferably at most about 22 wt% dill seed particles, and more preferably at most about 20 wt% dill seed particles. For example, the homogenized dill seed material of the aerosol-generating article according to the first preferred embodiment of the present invention comprises, on a dry weight basis, from about 2.5 wt% to about 25 wt% dill seed particles, or from about 4 wt% to about 24 wt% dill seed particles, or from about 5 wt% to about 23 wt% dill seed particles, or from about 6 wt% to about 22 wt% dill seed particles, or from about 8 wt% to about 21 wt% dill seed particles, or from about 10 wt% to about 20 wt% dill seed particles.
[0088] According to a second preferred embodiment of the present invention, the homogenized dill seed material comprises at most about 65% by weight of dill seed particles, more preferably at most about 60% by weight of dill seed particles, more preferably at most about 55% by weight of dill seed particles, more preferably at most about 50% by weight of dill seed particles, and more preferably at most about 45% by weight of dill seed particles. For example, the homogenized dill seed material of the aerosol-generating article according to the first preferred embodiment of the present invention comprises, on a dry weight basis, from about 2.5% to about 65% by weight of dill seed particles, or from about 10% to about 60% by weight of dill seed particles, or from about 15% to about 55% by weight of dill seed particles, or from about 20% to about 50% by weight of dill seed particles, or from about 30% to about 45% by weight of dill seed particles, or from about 35% to about 45% by weight of dill seed particles.
[0089] In certain embodiments of the present invention, the plant particles forming the homogenized dill seed material may comprise at least 98% by weight of dill seed particles, or at least 95% by weight of dill seed particles, or at least 90% by weight of dill seed particles, based on the dry weight of the plant particles. In such embodiments, the aerosol-generating substrate thus comprises dill seed particles and is substantially free of other plant particles. For example, the plant particles forming the homogenized dill seed material may comprise approximately 100% by weight of dill seed particles.
[0090] In an alternative embodiment of the invention, as described below, the homogenised dill seed material may comprise a combination of dill seed particles and tobacco particles.
[0091] In the following description of the invention, the terms "granular plant material" and "plant particles" are used collectively to refer to plant material particles used to form homogenised plant material. The granular plant material may consist essentially of dill seed particles or may be a mixture of dill seed particles and tobacco particles.
[0092] As noted above, the inventors have identified a number of "signature compounds" that are characteristic of the dill seed plant and therefore indicative of the inclusion of dill seed plant particles within the aerosol generating matrix.
[0093] It is expected that the amount of characteristic compounds present in pure dill seed particles will be different from the amount present in the aerosol-forming matrix. The process of preparing the matrix, which involves hydration in a slurry or suspension and drying at elevated temperatures, as well as the presence of other ingredients such as aerosol formers, will differentially alter the amount of each characteristic compound. The integrity of the dill seed particles and the stability of the compounds under temperature and manipulation during manufacturing will also affect the ultimate amount of the compounds present in the matrix. Therefore, it is expected that the ratios of the characteristic compounds relative to each other will be different after the dill seed particles are introduced into the matrix in various physical forms, such as sheets, strips, and granules.
[0094] The presence of dill seed in the aerosol-generating matrix and the proportion of dill seed provided in the aerosol-generating matrix can be determined by measuring the amount of a characteristic compound in the matrix and comparing it to the corresponding amount of the characteristic compound in pure dill seed material. The presence and amount of the characteristic compound can be determined using any suitable technique known to those skilled in the art.
[0095] In suitable technology, the sample of 250 milligrams of aerosol generation matrix is mixed with 5 milliliters of methanol, and extracted by vibration, vortex 5 minutes and centrifugation (4500g, 5 minutes, 10 degrees Celsius). The aliquot (300 microlitres) of the extract is transferred to a silanization chromatography bottle and diluted with methanol (600 microlitres) and internal standard (ISTD) solution (100 microlitres). The bottle is sealed and Eppendorf ThermoMixer (5 degrees Celsius; 2000rpm) is mixed for 5 minutes. The test sample from the obtained extract is analyzed by LC-HRAM-MS with the full scan mode of combination and data dependent fragmentation mode to identify characteristic compounds.
[0096] In some embodiments, the homogenized dill seed material further comprises up to about 75% by weight on a dry weight basis of tobacco particles.
[0097] For example, the homogenized dill seed material preferably comprises, on a dry weight basis, from about 10% to about 75% by weight tobacco particles, more preferably from about 15% to about 70% by weight tobacco particles, more preferably from about 20% to about 65% by weight tobacco particles, more preferably from about 25% to about 60% by weight tobacco particles, and more preferably from about 30% to about 70% by weight tobacco particles.
[0098] In some preferred embodiments, the homogenized dill seed material comprises, on a dry weight basis, from about 5% to about 20% by weight dill seed particles and from about 55% to about 70% by weight tobacco particles.
[0099] In the aerosol-generating article according to the first preferred embodiment of the present invention as defined above, the homogenized dill seed material preferably comprises, on a dry weight basis, from about 40% to about 75% by weight of tobacco particles, more preferably from about 45% to about 70% by weight of tobacco particles, and even more preferably from about 50% to about 65% by weight of tobacco particles. For example, the homogenized dill seed material according to the first embodiment may comprise, on a dry weight basis, from about 5% to about 20% by weight of dill seed particles and from about 55% to about 70% by weight of tobacco particles.
[0100] In the aerosol-generating article according to the second preferred embodiment of the present invention as defined above, the homogenized dill seed material preferably comprises, on a dry weight basis, from about 5 wt% to about 65 wt% tobacco particles, more preferably from about 10 wt% to about 60 wt% tobacco particles, and even more preferably from about 20 wt% to about 55 wt% tobacco particles. For example, the homogenized dill seed material according to the second embodiment may comprise, on a dry weight basis, from about 2.5 wt% to about 65 wt% dill seed particles and from about 1 wt% to about 65 wt% tobacco particles.
[0101] The weight ratio of dill seed particles to tobacco particles in the granular plant material forming the homogenized dill seed material can vary depending on the desired flavor profile and the composition of the aerosol. Preferably, the homogenized dill seed material comprises a weight ratio of dill seed particles to tobacco particles of no more than 1:4. This means that the dill seed particles comprise no more than 20% of the total granular plant material. More preferably, the homogenized dill seed material comprises a weight ratio of dill seed particles to tobacco particles of no more than 1:5, more preferably no more than 1:6.
[0102] For example, in a first preferred embodiment, the weight ratio of dill seed particles to tobacco particles is about 1:4. This 1:4 ratio corresponds to a granular plant material composed of about 20% by weight dill seed particles and about 80% by weight tobacco particles. For a homogenized dill seed material formed with about 75% by weight granular plant material, this corresponds to about 15% by weight dill seed particles and about 60% by weight tobacco particles in the homogenized dill seed material, based on dry weight.
[0103] In another embodiment, the homogenized dill seed material comprises dill seed particles to tobacco particles in a weight ratio of 1 :9. In yet another embodiment, the homogenized dill seed material comprises dill seed particles to tobacco particles in a weight ratio of 1 :30.
[0104] With reference to the present invention, term " tobacco particles " describes the particle of any plant member of Nicotiana.Term " tobacco particles " comprises ground or pulverized tobacco leaf blade, ground or pulverized tobacco leaf stem, tobacco dust, tobacco fines and other granular tobacco by-products that form in the processing, operation and transportation process of tobacco.In a preferred embodiment, tobacco particles are all derived from tobacco leaf blade basically.By contrast, isolated nicotine and nicotine salt are compounds that are derived from tobacco, but are not considered to tobacco particles for purposes of the present invention and are not included in the percentage of granular plant material.
[0105] Tobacco particles can be prepared by one or more tobacco plants. Any type of tobacco can be used in a blend. The example of spendable tobacco type includes but is not limited to sun-cured tobacco, flue-cured tobacco, burley tobacco, Maryland tobacco (Maryland tobacco), Oriental tobacco (Oriental tobacco), Virginia tobacco (Virginia tobacco) and other special tobaccos.
[0106] Flue-curing is a method of curing tobacco, particularly used with Virginia tobacco. During the curing process, heated air is circulated through densely packed tobacco. During the first stage, the tobacco leaves turn yellow and wilt. During the second stage, the leaves are completely dried. In the third stage, the stems are completely dried.
[0107] Burley tobacco plays an important role in many tobacco blends.Burley tobacco has a distinctive flavor and aroma, and also has the ability to absorb large amounts of casing.
[0108] Oriental tobacco is a type of tobacco with small leaves and high aromatic qualities. However, the flavor of Oriental tobacco is milder than, for example, Burley tobacco. Therefore, a relatively small proportion of Oriental tobacco is typically used in tobacco blends.
[0109] Kasturi, Madura and Jatim are all subtypes of sun-cured tobacco that can be used. Preferably, Kasturi tobacco and flue-cured tobacco can be used in a mixture to produce tobacco particles. Therefore, the tobacco particles in the granular plant material can include a mixture of Kasturi tobacco and flue-cured tobacco.
[0110] The tobacco particles may have a nicotine content of at least about 2.5% by weight on a dry weight basis. More preferably, the tobacco particles may have a nicotine content of at least about 3% by weight, even more preferably at least about 3.2% by weight, even more preferably at least about 3.5% by weight, and most preferably at least about 4% by weight on a dry weight basis. When the aerosol-generating substrate contains a combination of tobacco particles and dill seed particles, it is preferred to use tobacco with a higher nicotine content to maintain a nicotine level similar to that of a typical aerosol-generating substrate without dill seed particles, because otherwise the total amount of nicotine will be reduced due to the replacement of tobacco particles with dill seed particles.
[0111] Because of the inclusion of tobacco particles, the aerosol-generating substrate of such embodiments and the aerosol generated therefrom contain a proportion of tobacco's “signature compounds.” Signature compounds generated by tobacco include, but are not limited to, anatabine, cotinine, and damascenone.
[0112] Nicotine can optionally be introduced into the aerosol-generating matrix, but for the purposes of the present invention, this will be considered a non-tobacco material. Nicotine can comprise one or more nicotine salts selected from the following list: nicotine lactate, nicotine citrate, nicotine pyruvate, nicotine bitartrate, nicotine benzoate, nicotine pectinate, nicotine alginate and nicotine salicylate. In addition to tobacco with a low nicotine content, nicotine can also be introduced, or nicotine can be introduced into an aerosol-generating matrix with a reduced tobacco content or a zero tobacco content.
[0113] In certain embodiments of the invention, the aerosol-generating substrate comprises a homogenised dill seed material formed from particulate plant material consisting solely of dill seed particles, wherein nicotine, such as a nicotine salt, is introduced into the aerosol-generating substrate.
[0114] Preferably, the aerosol-generating substrate comprises at least about 0.1 mg of nicotine per gram of substrate by dry weight. More preferably, the aerosol-generating substrate comprises at least about 0.5 mg of nicotine per gram of substrate, more preferably at least about 1 mg of nicotine per gram of substrate, more preferably at least about 1.5 mg of nicotine per gram of substrate, more preferably at least about 2 mg of nicotine per gram of substrate, more preferably at least about 3 mg of nicotine per gram of substrate, more preferably at least about 4 mg of nicotine per gram of substrate, more preferably at least about 5 mg of nicotine per gram of substrate.
[0115] Preferably, the aerosol-generating substrate comprises at most about 50 mg of nicotine per gram of substrate by dry weight. More preferably, the aerosol-generating substrate comprises at most about 45 mg of nicotine per gram of substrate, more preferably at most about 40 mg of nicotine per gram of substrate, more preferably at most about 35 mg of nicotine per gram of substrate, more preferably at most about 30 mg of nicotine per gram of substrate, more preferably at most about 25 mg of nicotine per gram of substrate, more preferably at most about 20 mg of nicotine per gram of substrate.
[0116] For example, the aerosol-generating substrate may comprise, by dry weight, from about 0.1 mg to about 50 mg of nicotine per gram of substrate, or from about 0.5 mg to about 45 mg of nicotine per gram of substrate, or from about 1 mg to about 40 mg of nicotine per gram of substrate, or from about 2 mg to about 35 mg of nicotine per gram of substrate, or from about 5 mg to about 30 mg of nicotine per gram of substrate, or from about 10 mg to about 25 mg of nicotine per gram of substrate, or from about 15 mg to about 20 mg of nicotine per gram of substrate. In certain preferred embodiments of the present invention, the aerosol-generating substrate comprises, by dry weight, from about 1 mg to about 20 mg of nicotine per gram of substrate.
[0117] The defined ranges for the nicotine content of the aerosol-generating substrate include all forms of nicotine that may be present in the aerosol-generating substrate, including nicotine inherently present in the tobacco material and nicotine that has optionally been separately added to the aerosol-generating substrate, for example in the form of a nicotine salt.
[0118] For example, the particulate plant material may comprise, more preferably, from about 45% to about 60% by weight tobacco particles, and more preferably from about 50% to about 65% by weight tobacco particles on a dry weight basis.
[0119] In addition to the dill seed particles or the combination of dill seed particles and tobacco particles ("granular plant material"), the homogenized dill seed material may also contain a proportion of other plant flavor particles.
[0120] For the purposes of the present invention, the term "other plant flavor particles" refers to particles of non-dill seed, non-tobacco, and non-cannabis plant materials that are capable of generating one or more flavoring agents upon heating. This term should be construed to exclude particles of inert plant materials, such as cellulose, that do not contribute to the sensory output of the aerosol-forming matrix. The particles may be ground or pulverized leaves, fruits, stems, stalks, roots, seeds, buds, or bark of other plants. Suitable plant flavor particles for inclusion in an aerosol-forming matrix according to the present invention will be known to those skilled in the art and include, but are not limited to, clove particles and tea particles.
[0121] By blending the desired amounts and types of different plant particles, the composition of the homogenized dill seed material can be advantageously adjusted. This enables the aerosol-generating matrix to be formed from a single homogenized dill seed material, if desired, without the need to combine or mix different blends, such as is the case in the production of conventional shredded fillers. Thus, the production of the aerosol-generating matrix can potentially be simplified.
[0122] The particulate plant material used in the aerosol generating matrix of the present invention can be adapted to provide a desired particle size distribution. The particle size distribution is expressed herein as a D-value, where the D-value refers to the percentage by number of particles having a diameter less than or equal to a given D-value. For example, in a D95 particle size distribution, 95% by number of the particles have a diameter less than or equal to a given D95 value, and 5% by number of the particles have a diameter greater than a given D95 value. Similarly, in a D5 particle size distribution, 5% by number of the particles have a diameter less than or equal to the D5 value, and 95% by number of the particles have a diameter greater than a given D5 value. The D5 and D95 values combined therefore provide an indication of the particle size distribution of the particulate plant material.
[0123] The granular plant material can have a D95 value ranging from greater than or equal to 200 microns to a D95 value less than or equal to 1000 microns. This means that the granular plant material can have a distribution represented by any D95 value within a given range, i.e., D95 can be equal to 200 microns, or D95 can be equal to 250 microns, and so on, all the way up to D95 can be equal to 1000 microns. By providing D95 values within this range, the inclusion of relatively large plant particles in the homogenized dill seed material is avoided. This is desirable because aerosol generation from such large plant particles can be relatively inefficient. Furthermore, the inclusion of large plant particles in the homogenized dill seed material can adversely affect the consistency of the material.
[0124] Preferably, the particulate plant material can have a D95 value of greater than or equal to about 200 microns to a D95 value of less than or equal to about 900 microns, more preferably a D95 value of greater than or equal to about 300 microns to a D95 value of less than or equal to about 800 microns. Both the particulate dill seed material and the particulate tobacco material can have a D95 value of greater than or equal to about 20 microns to a D95 value of less than or equal to about 1000 microns, preferably a D95 value of greater than or equal to 200 microns to a D95 value of less than or equal to about 900 microns, more preferably a D95 value of greater than or equal to about 300 microns to a D95 value of less than or equal to about 800 microns.
[0125] Preferably, the particulate plant material can have a D5 value of greater than or equal to about 10 microns to a D5 value of less than or equal to about 50 microns, more preferably a D5 value of greater than or equal to about 20 microns to a D5 value of less than or equal to about 40 microns. By providing a D5 value within this range, inclusion of very small dust particles in the homogenized dill seed material can be avoided, which can be desirable from a manufacturing perspective.
[0126] In some embodiments, the granular plant material can be purposefully ground to form particles having a desired particle size distribution.Using purposefully ground plant material advantageously improves the uniformity of the granular plant material and the consistency of the homogenized dill seed material.
[0127] 100% of the particulate plant material may have a diameter of less than or equal to about 2000 microns, more preferably less than or equal to about 1500 microns. 100% of the particulate dill seed material and 100% of the particulate tobacco material may have a diameter of less than or equal to about 2000 microns, more preferably less than or equal to about 1500 microns. The size range of the dill seed particles enables the dill seed particles to be combined with tobacco particles in existing cast leaf processes.
[0128] The homogenized dill seed material preferably comprises at least about 55% by weight, on a dry weight basis, of granular plant material comprising dill seed particles as described above, more preferably at least about 60% by weight of granular plant material, and even more preferably at least about 65% by weight of granular plant material. The homogenized dill seed material preferably comprises no more than about 95% by weight, on a dry weight basis, more preferably no more than about 90% by weight of granular plant material, and even more preferably no more than about 85% by weight of granular plant material. For example, the homogenized dill seed material may comprise from about 55% to about 95% by weight, on a dry weight basis, of granular plant material, or from about 60% to about 90% by weight of granular plant material, or from about 65% to about 85% by weight of granular plant material. In a particularly preferred embodiment, the homogenized dill seed material comprises about 75% by weight, on a dry weight basis, of granular plant material.
[0129] Preferably, the total weight amount of particulate plant material in the homogenized dill seed material of the first preferred embodiment does not exceed about 75% by weight on a dry weight basis.
[0130] Preferably, the total weight amount of particulate plant material in the homogenized dill seed material of the second preferred embodiment does not exceed about 75% by weight on a dry weight basis, or does not exceed about 65% by weight on a dry weight basis.
[0131] Thus, the particulate plant material is combined with one or more other components to form a homogenised dill seed material.
[0132] As defined above, the homogenized dill seed material also includes an aerosol former. Upon volatilization, the aerosol former can transport other vaporized compounds released from the aerosol-forming substrate upon heating, such as nicotine and flavorings, in the aerosol. The aerosolization of a particular compound from an aerosol-forming substrate is not solely determined by its boiling point. The amount of aerosolized compound can be affected by the physical form of the substrate and other components also present in the substrate. The stability of the compound under the temperature and time range of aerosolization will also affect the amount of the compound present in the aerosol.
[0133] Suitable aerosol formers for inclusion in the homogenized dill seed material are known in the art and include, but are not limited to: polyols, such as triethylene glycol, 1,3-butylene glycol, and glycerol; esters of polyols, such as glycerol mono-, di-, or triacetate; and fatty acid esters of mono-, di-, or polycarboxylic acids, such as dimethyl dodecanedioate and dimethyl tetradecanedioate. The homogenized dill seed material may contain a single aerosol former, or a combination of two or more aerosol formers.
[0134] If the substrate is intended for use in an aerosol-generating article of an electrically operated aerosol-generating system having a heating element, the aerosol-former is preferably glycerol.
[0135] The amount of aerosol-former can be adjusted depending on the composition of the homogenized dill seed material, such as the type or amount of plant particles, in order to obtain an aerosol having a desired level of flavor compounds from the plant particles. The amount of aerosol-former can also be adjusted depending on the manner in which the aerosol-generating substrate is intended to be heated during use, in particular the temperature to which the aerosol-generating substrate will be heated during heating of the aerosol-generating article in an associated aerosol-generating device.
[0136] The homogenized dill seed material preferably has an aerosol former content of from about 5 wt% to about 55 wt% on a dry weight basis, such as from about 10 wt% to about 45 wt% on a dry weight basis, or from about 15 wt% to about 40 wt% on a dry weight basis.
[0137] The aerosol-forming agent content may be between about 5% and about 30% by weight on a dry weight basis. For example, in the homogenized dill seed material according to the first preferred embodiment of the present invention as defined above, the aerosol-forming agent content, on a dry weight basis, is preferably between about 5% and about 30% by weight, more preferably between about 10% and about 25% by weight, and even more preferably between about 15% and about 20% by weight.
[0138] Alternatively, the aerosol-forming agent content may be between about 15 wt% and about 55 wt% on a dry weight basis. For example, in the homogenized dill seed material according to the second preferred embodiment of the present invention as defined above, the aerosol-forming agent content, on a dry weight basis, is preferably between about 15 wt% and about 55 wt%, more preferably between about 25 wt% and about 50 wt%, and even more preferably between about 35 wt% and about 45 wt%.
[0139] In other embodiments, the homogenized dill seed material may have an aerosol-forming agent content of about 1% to about 5% by weight on a dry weight basis. For example, if the substrate is intended for use in an aerosol-generating article in which the aerosol-forming agent is retained in a reservoir separate from the substrate, the substrate may have an aerosol-forming agent content of greater than 1% and less than about 5%. In such embodiments, the aerosol-forming agent volatilizes upon heating, and the stream of aerosol-forming agent contacts the aerosol-generating substrate to entrain flavor from the aerosol-generating substrate in the aerosol.
[0140] The aerosol-forming agent may act as a humectant in the aerosol-generating matrix.
[0141] As defined above, the homogenized dill seed material further comprises a binder to modify the mechanical properties of the granular plant material, wherein the binder is included in the homogenized dill seed material during manufacture as described herein. Suitable exogenous binders are known to those skilled in the art and include, but are not limited to, gums such as guar gum, xanthan gum, gum arabic, and locust bean gum; cellulosic binders such as cellulose ethers such as hydroxypropyl cellulose, carboxymethyl cellulose (CMC), hydroxyethyl cellulose, methyl cellulose, and ethyl cellulose; polysaccharides such as starch; organic acids such as alginic acid; conjugate base salts of organic acids such as sodium alginate, agar, and pectin; and combinations thereof. Preferably, the binder comprises guar gum.
[0142] Preferably, the binder is present in an amount of about 1 wt% to about 10 wt%, preferably about 2 wt% to about 9 wt%, more preferably about 3 wt% to about 8 wt%, on a dry weight basis.
[0143] In certain embodiments, the homogenized dill seed material preferably comprises from about 1% to about 10% by weight of a binder, on a dry weight basis, wherein the binder is most preferably guar gum. For example, in an aerosol-generating article according to the first preferred embodiment of the present invention as defined above, the homogenized dill seed material preferably comprises from about 1% to about 10% by weight of a binder, on a dry weight basis, wherein the binder is most preferably guar gum. For example, the homogenized dill seed material of the first preferred embodiment may comprise from about 2.5% to about 25% by weight of dill seed particles, from about 5% to about 30% by weight of an aerosol-forming agent, and from about 1% to about 10% by weight of a binder.
[0144] In certain embodiments, the homogenized dill seed material preferably comprises from about 2% to about 10% by weight of a binder, based on dry weight, wherein the binder is most preferably a cellulose ether. For example, in an aerosol-generating article according to the second preferred embodiment as defined above, the homogenized dill seed material preferably comprises from about 2% to about 10% by weight of a binder, based on dry weight, wherein the binder is preferably a cellulose ether. Particularly preferably, the binder is carboxymethylcellulose (CMC). For example, the homogenized dill seed material of the second preferred embodiment may comprise from about 2.5% to about 65% by weight of dill seed particles, from about 15% to about 55% by weight of an aerosol-forming agent, and from about 2% to about 10% by weight of a cellulose ether.
[0145] Additionally, the homogenized dill seed material of any embodiment may optionally further comprise additional cellulose. For example, the homogenized dill seed material may comprise from about 5% to about 50% by weight of additional cellulose.
[0146] As used herein, the term "additional cellulose" encompasses any cellulose material introduced into the homogenized dill seed material that is not derived from the dill seed particles or tobacco particles provided in the homogenized dill seed material. Thus, in addition to the dill seed plant material or tobacco material, the additional cellulose is introduced into the homogenized dill seed material as a separate and distinct cellulose source from any cellulose inherently provided within the dill seed particles or tobacco particles. The additional cellulose is typically derived from a different plant than the dill seed particles or tobacco particles. Preferably, the additional cellulose is in the form of an inert cellulose material that is sensorily inert and therefore does not substantially affect the organoleptic properties of the aerosol generated by the aerosol generating substrate. For example, the additional cellulose is preferably a tasteless and odorless material.
[0147] The additional cellulose may consist of one type of cellulosic material, or may be a combination of different types of cellulosic materials that provide different properties, as described in more detail below.
[0148] The additional cellulose incorporated into the homogenised dill seed material forming the aerosol-generating substrate of aerosol-generating articles according to the invention is believed to provide additional structure and reinforcement to bind and support the plant particles and aerosol-former within the homogenised material.
[0149] In homogenized dill seed materials wherein the binder comprises a cellulose ether as described above, the introduction of additional cellulose has been found to be particularly beneficial. It has advantageously been found that combining the cellulose ether and the additional cellulosic material at certain defined levels and within defined ratios as set forth below provides a homogenized dill seed material having improved tensile strength and homogeneity.
[0150] Using certain types of binder materials, it can be technically difficult to produce a homogenized dill seed material with acceptable tensile strength when the proportion of dill seed particles is above a certain level. Using some binder materials, above a threshold level of dill seed particles, the homogenized dill seed material has been found to have low tensile strength and an uneven texture. If the tensile strength of the homogenized dill seed material is too low, it is brittle and cannot be effectively processed to form an aerosol-generating substrate, particularly on an industrial scale.
[0151] The inventors of the present application have discovered that by using a specific combination of cellulose ether and additional cellulose in a homogenized dill seed material as defined above, more effective dill seed particle binding can be achieved and the resulting homogenized dill seed material has significantly higher tensile strength. Consequently, the resulting homogenized dill seed material can be readily processed into an aerosol-generating substrate using existing high-speed equipment and techniques.
[0152] Preferably, the ratio of additional cellulosic material to cellulose ether in the homogenised dill seed material is at least 2.
[0153] Preferably, the additional cellulose comprises cellulose powder. As used herein, the term "cellulose powder" refers to a refined cellulose material in powder form derived from cellulose fibers. Preferably, the cellulose powder is formed from particles having an average particle size of less than 100 microns. The cellulose powder may be in the form of microcrystalline cellulose. Cellulose powder suitable for use in the present invention may be obtained from Gumix International, Inc. of New Jersey as Microcrystalline Cellulose Type SK-105 or SK-101 or Cellulose Powder Type M-60.
[0154] Preferably, the amount of cellulose powder corresponds to at least about 5% by weight of the homogenized dill seed material, more preferably at least about 6% by weight of the homogenized dill seed material, more preferably at least about 7% by weight of the homogenized dill seed material, more preferably at least about 8% by weight of the homogenized dill seed material, based on dry weight.
[0155] The amount of cellulose powder can be adjusted above this minimum level depending on the weight of other components in the homogenized dill seed material, particularly the weight of the plant particles. In certain embodiments, cellulose powder can replace a certain proportion of the plant particles in the homogenized dill seed material without significantly affecting the properties of the generated aerosol.
[0156] Preferably, the amount of cellulose powder corresponds to no more than about 45% by weight of the homogenized dill seed material, more preferably no more than about 40% by weight of the homogenized dill seed material, on a dry weight basis.
[0157] In certain embodiments, for example, in embodiments having relatively high levels of particulate plant material in the homogenized dill seed material, the amount of cellulose powder can be relatively low. In such embodiments, the amount of cellulose powder can be between about 5% and about 15% by weight of the homogenized dill seed material, or between about 6% and about 12% by weight of the homogenized dill seed material, or between about 7% and about 11% by weight of the homogenized dill seed material, or between about 8% and about 10% by weight of the homogenized dill seed material, on a dry weight basis.
[0158] In other embodiments, for example, in embodiments having relatively low levels of particulate plant material in the homogenized dill seed material, the amount of cellulose powder can be relatively higher. In such embodiments, the amount of cellulose powder can be between about 15% and about 45% by weight of the homogenized dill seed material, or between about 20% and about 40% by weight of the homogenized dill seed material, or between about 25% and about 35% by weight of the homogenized dill seed material, on a dry weight basis.
[0159] Preferably, where the homogenized dill seed material comprises a cellulose ether and a cellulose powder, the weight ratio of the cellulose powder to the cellulose ether in the homogenized plant material is at least about 1.5, i.e., the amount of cellulose powder is at least 1.5 times the amount of cellulose ether. More preferably, the weight ratio of the cellulose powder to the cellulose ether in the homogenized dill seed material is at least about 1.6, and more preferably at least about 1.8.
[0160] As an alternative to or in addition to cellulose powder, additional cellulose may include cellulose fibers. As used herein, the term "cellulose fibers" refers to fibers obtained directly from plant-based materials, wherein the length of each fiber is significantly greater than its width. The cellulose fibers preferably have a fiber length of at least 400 microns. Cellulose fibers suitable for use in the present invention include, for example, wood pulp fibers. A suitable source of cellulose fibers for use in the present invention can be obtained from Storaenso, Sweden, as ECF bleached hardwood kraft pulp.
[0161] Cellulose fibers may advantageously serve as mechanical reinforcement in the homogenized dill seed material forming the aerosol-generating substrate of an aerosol-generating article according to the present invention. Cellulose fibers may improve the binding of plant particles in the homogenized dill seed material and provide improved tensile strength, particularly when combined with a cellulose ether binder.
[0162] Preferably, the amount of cellulose fibers corresponds to at least about 3% by weight of the homogenized dill seed material on a dry weight basis, more preferably at least about 4% by weight of the homogenized dill seed material on a dry weight basis, more preferably at least about 5% by weight of the homogenized dill seed material, more preferably at least about 6% by weight of the homogenized dill seed material.
[0163] Preferably, the amount of cellulose fiber corresponds to no more than about 12% by weight of the homogenized dill seed material, more preferably at least about 11% by weight of the homogenized dill seed material, more preferably at least about 10% by weight of the homogenized dill seed material, and more preferably at least about 8% by weight of the homogenized dill seed material, on a dry weight basis.
[0164] For example, on a dry weight basis, the homogenized dill seed material can comprise from about 3% to about 12% cellulose fibers, or from about 4% to about 11% cellulose fibers, or from about 5% to about 10% cellulose fibers, or from about 6% to about 8% cellulose fibers.
[0165] Preferably, where the homogenized dill seed material comprises cellulose ether and cellulose fibers, the weight ratio of cellulose fibers to cellulose ether in the homogenized dill seed material is at least about 0.5, i.e., the amount of cellulose powder is at least half the amount of cellulose ether. More preferably, the weight ratio of cellulose fibers to cellulose ether in the homogenized dill seed material is at least about 0.75, and even more preferably at least about 1.
[0166] In a preferred embodiment, the additional cellulose comprises cellulose powder and cellulose fibers. In such an embodiment, the weight ratio of cellulose powder to cellulose fibers is preferably at least about 1.5, more preferably at least about 1.75, and more preferably at least about 2.
[0167] Preferably, the amount of additional cellulose provided in the homogenized dill seed material is adjusted so that the total amount of additional cellulose and plant particles corresponds to no more than 75% by weight of the homogenized dill seed material. Preferably, at least about 25% by weight of the homogenized dill seed material is thus provided by other components, including the cellulose ether and the aerosol former.
[0168] In the aerosol-generating article according to the second preferred embodiment of the present invention, the homogenized dill seed material preferably comprises, on a dry weight basis, from about 2 wt% to about 10 wt% cellulose ether and from about 5 wt% to about 50 wt% additional cellulose. Preferably, the ratio of additional cellulose to cellulose ether is at least 2.
[0169] For example, the homogenized dill seed material according to the second preferred embodiment of the present invention may comprise: 2.5% to 75% by weight of dill seed particles, based on dry weight; 15% to 55% by weight of aerosol former, based on dry weight; 2% to 10% by weight of cellulose ether, based on dry weight; and 3% to 50% by weight of additional cellulose, based on dry weight. Such homogenized dill seed material preferably also comprises at least 1% by weight of tobacco particles, based on dry weight.
[0170] In addition to the above components, the homogenized dill seed material can optionally further comprise one or more lipids to facilitate diffusion of volatile components (e.g., aerosol formers, (E)-anethole, and nicotine), wherein the lipids are included in the homogenized plant material during manufacture as described herein. Suitable lipids for inclusion in the homogenized dill seed material include, but are not limited to, medium-chain triglycerides, cocoa butter, palm oil, palm kernel oil, mango butter, shea butter, soybean oil, cottonseed oil, coconut oil, hydrogenated coconut oil, candelilla wax, carnauba wax, shellac, sunflower wax, sunflower oil, rice bran, and Revel A; and combinations thereof.
[0171] Alternatively or additionally, the homogenized dill seed material may further comprise a pH adjusting agent.
[0172] Alternatively or additionally, the homogenized dill seed material may further comprise fibers to modify the mechanical properties of the homogenized dill seed material, wherein the fibers are included in the homogenized dill seed material during manufacture as described herein. Suitable exogenous fibers for inclusion in the homogenized dill seed material are known in the art and include fibers formed from non-tobacco materials and non-dill seed materials, including but not limited to: cellulose fibers; softwood fibers; hardwood fibers; jute fibers, and combinations thereof. Exogenous fibers derived from tobacco and / or dill seed may also be added. Any fibers added to the homogenized dill seed material are not considered to form part of the "granular plant material" as defined above. Prior to inclusion in the homogenized dill seed material, the fibers may be processed by suitable methods known in the art, including but not limited to: mechanical pulping; refining; chemical pulping; bleaching; sulfate pulping; and combinations thereof. The fibers typically have a length greater than their width.
[0173] Suitable fibers typically have a length greater than 400 microns and less than or equal to 4 mm, preferably in the range of 0.7 mm to 4 mm. Preferably, the fibers are present in an amount of at least about 2% by weight, based on the dry weight of the substrate. The amount of fiber in the homogenized dill seed material may depend on the type of material and, in particular, the method used to produce the homogenized dill seed material. In some embodiments, the fibers may be present in an amount of about 2% to about 15% by weight, most preferably about 4% by weight, based on the dry weight of the substrate. For example, such levels of fiber may be present when the homogenized plant material is in the form of cast leaves. In other embodiments, the fibers may be present in an amount of at least about 30% by weight or at least about 40% by weight. For example, such higher levels of fiber may be provided when the homogenized dill seed material is dill seed paper formed in a papermaking process.
[0174] In a preferred embodiment of the present invention, the homogenized dill seed material comprises dill seed particles, from about 5% to about 30% by weight of an aerosol former, and from about 1% to about 10% by weight of a binder, based on dry weight. In such an embodiment, the homogenized dill seed material preferably also comprises from about 2% to about 15% by weight of fiber. Particularly preferably, the binder is guar gum.
[0175] The homogenized plant material of the aerosol-generating substrate according to the present invention can comprise a single type of homogenized plant material or two or more types of homogenized plant material having different compositions or forms. For example, in one embodiment, the aerosol-generating substrate comprises dill seed particles and tobacco particles contained within the same sheet of homogenized plant material. However, in other embodiments, the aerosol-generating substrate can comprise tobacco particles and dill seed particles within different sheets.
[0176] The homogenised dill seed material is preferably in the form of a solid or gel. However, in some embodiments, the homogenised material may be in the form of a solid that is not a gel. Preferably, the homogenised material is not in the form of a film.
[0177] The homogenized dill seed material may be provided in any suitable form. For example, the homogenized dill seed material may be in the form of one or more sheets. As used herein with reference to the present invention, the term "sheet" describes a laminar element having a width and length substantially greater than its thickness.
[0178] Alternatively or additionally, the homogenized dill seed material may be in the form of a plurality of pellets or granules.
[0179] Alternatively or additionally, the homogenised dill seed material may be in a form that can be filled into a cigarette cartridge or hookah consumable, or can be used in a hookah device.The present invention includes a cigarette cartridge or hookah device containing the homogenised dill seed material.
[0180] Alternatively or additionally, the homogenized dill seed material may be in the form of a plurality of strips, shreds, or fragments. As used herein, the term "strip" describes an elongated element of material whose length is substantially greater than its width and thickness. The term "strip" should be considered to include ribbons, fragments, and any other homogenized dill seed material having similar forms. The strips of homogenized dill seed material may be formed from a sheet of homogenized dill seed material, for example, by cutting or chopping, or by other methods, such as by extrusion.
[0181] In some embodiments, the strips may be formed in situ within the aerosol-generating substrate due to the splitting or cracking of the sheet of homogenized dill seed material during the formation of the aerosol-generating substrate, for example due to curling. The strips of homogenized dill seed material within the aerosol-generating substrate may be separated from each other. Alternatively, each strip of homogenized dill seed material within the aerosol-generating substrate may be at least partially connected to one or more adjacent strips along the length of the strip. For example, adjacent strips may be connected by one or more fibers. This may occur, for example, when the strips are formed due to the splitting of the sheet of homogenized dill seed material during the production of the aerosol-generating substrate, as described above.
[0182] Preferably, the aerosol generating substrate is in the form of one or more sheets of homogenized dill seed material. In various embodiments of the present invention, the one or more sheets of homogenized dill seed material can be produced by a casting process. In various embodiments of the present invention, the one or more sheets of homogenized dill seed material can be produced by a papermaking process. The one or more sheets as described herein can each individually have a thickness between 100 microns and 600 microns, preferably between 150 microns and 300 microns, and most preferably between 200 microns and 250 microns. Individual thickness refers to the thickness of an individual sheet, while combined thickness refers to the total thickness of all sheets that make up the aerosol generating substrate. For example, if the aerosol generating substrate is formed by two individual sheets, the combined thickness is the sum of the thicknesses of the two individual sheets or, if two sheets are stacked in the aerosol generating substrate, the measured thickness of the two sheets.
[0183] One or more sheets as described herein may each individually have a density of about 100 g / m 2 About 300g / m 2 Gram weight per square meter.
[0184] One or more sheets as described herein may each individually have a viscosity of about 0.3 g / cm 3 to about 1.3g / cm 3 , preferably about 0.7 g / cm 3 to about 1.0g / cm 3 density.
[0185] The term "tensile strength" is used throughout this specification to refer to a measure of the force required to stretch a sheet of homogenized dill seed material until it breaks. More specifically, tensile strength is the maximum tensile force per unit width that the sheet material will withstand before breaking, and is measured in the longitudinal or transverse direction of the sheet material. The unit of expression for tensile strength is Newtons per meter (N / m). Methods for measuring the tensile strength of sheet materials are well known. A suitable test is described in the international standard ISO 1924-2, published in 2014, entitled "Paper and Board—Determination of Tensile Properties—Part 2: Constant Rate of Elongation Method."
[0186] The materials and equipment required for testing according to ISO 1924-2 are: a universal tension / compression testing machine, Instron 5566, or equivalent; a 100 Newton tension load cell, Instron or equivalent; two pneumatic grips; a steel gauge block 180 ± 0.25 mm long (width: approximately 10 mm, thickness: approximately 3 mm); a double-blade strip cutter, measuring 15 ± 0.05 × approximately 250 mm, Adamel Lhomargy, or equivalent; a scalpel; a computer running acquisition software Merlin, or equivalent; and compressed air.
[0187] Prepare the specimens by conditioning a homogenized sheet of dill seed material at 22 ± 2 degrees Celsius and 60 ± 5% relative humidity for at least 24 hours before testing. Then, cut the specimens longitudinally or transversely to approximately 250 x 15 ± 0.1 mm using a double-blade strip cutter. The specimens must be cut cleanly at the edges, so no more than three specimens should be cut simultaneously.
[0188] The tensile / compression testing apparatus was set up by installing a 100 Newton tension load cell, connecting a universal tensile / compression testing machine and a computer, and selecting the measurement method specified in the software. The test speed was set to 8 mm / min. The tension load cell was then calibrated and the pneumatic grips were installed. The test distance between the pneumatic grips was adjusted to 180 ± 0.5 mm using steel gauge blocks, and the distance and force were set to zero.
[0189] Then, place the specimen straight and centered between the grips, avoiding touching the test area with your fingers. Close the upper grip and suspend the paper strip in the open lower grip. Set the force to zero. Then, gently pull the paper strip downwards and close the lower grip; the initial force must be between 0.05 Newtons and 0.20 Newtons. As the upper grip moves upward, apply gradually increasing force until the specimen breaks. Repeat the same procedure for the remaining specimens. The result is valid if the specimen breaks when the grips are separated by more than 10 mm. If this is not the case, reject the result and perform additional measurements.
[0190] As mentioned above, if the available test specimens of homogenized dill seed material are smaller than those described in the test according to ISO 1924-2, the test can be easily scaled down to accommodate the available size of the test specimen.
[0191] One or more sheets of homogenized dill seed material as described herein can each individually have a peak tensile strength in the cross direction of 50 N / m to 400 N / m, or preferably 150 N / m to 350 N / m. Given that sheet thickness affects tensile strength, and where a batch of sheets exhibits thickness variation, it may be desirable to normalize this value to a specific sheet thickness.
[0192] One or more sheets as described herein can each individually have a peak tensile strength in the machine direction of 100 N / m to 800 N / m, or preferably 280 N / m to 620 N / m, normalized to a sheet thickness of 215 μm. The machine direction refers to the direction in which the sheet material is wound onto or unwound from a reel and fed into a machine, while the transverse direction is perpendicular to the machine direction. These tensile strength values make the sheets and methods described herein particularly suitable for subsequent operations involving mechanical stress.
[0193] Providing a sheet having thickness, grammage and tensile strength levels as defined above advantageously optimises the machinability of the sheet to form the aerosol-generating substrate and ensures that damage, such as tearing of the sheet, is avoided during high speed processing of the sheet.
[0194] In embodiments of the present invention in which the aerosol-generating substrate comprises one or more sheets of homogenized dill seed material, the sheets are preferably in the form of one or more gathered sheets. As used herein, the term "gathered" means that the sheets of homogenized dill seed material are rolled, folded, or otherwise compressed or condensed to be substantially transverse to the cylindrical axis of the rod or strip. The step of "gathering" the sheets can be performed by any suitable means that provides the necessary transverse compression of the sheets.
[0195] As used herein, the term "longitudinal" refers to a direction corresponding to the principal longitudinal axis of the aerosol-generating article, extending between the upstream and downstream ends of the aerosol-generating article. During use, air is drawn through the aerosol-generating article in the longitudinal direction. The term "transverse" refers to a direction perpendicular to the longitudinal axis. As used herein, the term "length" refers to the dimension of a component in the longitudinal direction, and the term "width" refers to the dimension of a component in the transverse direction. For example, in the case of a rod or strip having a circular cross-section, the maximum width corresponds to the diameter of the circle.
[0196] As used herein, the term "rod" refers to a generally cylindrical element having a substantially polygonal, circular, oval, or elliptical cross-section. As used herein, the term "strip" refers to a generally cylindrical element having a substantially polygonal cross-section, and preferably a circular, oval, or elliptical cross-section. The length of a strip can be greater than or equal to the length of a rod. Typically, the length of a strip is greater than the length of a rod. A strip can include one or more rods, preferably aligned longitudinally.
[0197] As used herein, the terms "upstream" and "downstream" describe the relative position of an element or portion of an element of an aerosol-generating article with respect to the direction in which the aerosol is transported through the aerosol-generating article during use. The downstream end of the airflow path is the end at which the aerosol is delivered to the user of the article.
[0198] One or more sheets of homogenized dill seed material can be gathered transversely relative to their longitudinal axis and confined with a wrapper to form a continuous strip or stick. The continuous strip can be cut into a plurality of discrete strips or sticks. The wrapper can be a paper wrapper or a non-paper wrapper, as described in more detail below.
[0199] Alternatively, one or more sheets of homogenized dill seed material can be cut into strips as described above. In such embodiments, the aerosol-generating substrate comprises a plurality of homogenized dill seed material strips. The strips can be used to form rods. Typically, the width of such strips is at least about 0.2 mm, or at least about 0.5 mm. Typically, the width of such strips does not exceed about 5 mm, or about 4 mm, or about 3 mm, or about 1.5 mm. For example, the width of the strips can be between about 0.25 mm and about 5 mm, or between about 0.25 mm and about 3 mm, or between about 0.5 mm and about 1.5 mm.
[0200] The length of the strips is preferably greater than about 5mm, for example, between about 5mm and about 20mm, or between about 8mm and about 15mm, or about 12mm. Preferably, the strips have substantially the same length as each other. The length of the strips can be determined by the manufacturing process, whereby the strips are cut into shorter rods, and the length of the strips corresponds to the length of the rod. The strips may be fragile, which may result in fracture, especially during transportation. In this case, the length of some strips may be less than the length of the rod.
[0201] The plurality of strips preferably extend substantially longitudinally along the length of the aerosol-generating substrate, aligned with the longitudinal axis. Preferably, the plurality of strips are therefore aligned substantially parallel to each other.
[0202] The strips of homogenized dill seed material preferably each have a mass to surface area ratio of at least about 0.02 milligrams per square millimeter, more preferably at least about 0.05 milligrams per square millimeter. Preferably, the strips of homogenized dill seed material each have a mass to surface area ratio of no more than about 0.2 milligrams per square millimeter, more preferably no more than about 0.15 milligrams per square millimeter. The mass to surface area ratio is calculated by dividing the mass of the strip of homogenized dill seed material (in milligrams) by the geometric surface area of the strip of homogenized dill seed material (in square millimeters).
[0203] The one or more sheets of homogenized dill seed material may be textured by crimping, embossing, or perforating. The one or more sheets may be textured prior to being gathered or prior to being cut into thin strips. Preferably, the one or more sheets of homogenized dill seed material are crimped prior to being gathered so that the homogenized dill seed material may be in the form of a crimped sheet, more preferably in the form of a gathered crimped sheet. As used herein, the term "crimped sheet" means a sheet having a plurality of substantially parallel ridges or corrugations generally aligned with the longitudinal axis of the article.
[0204] In one embodiment, the aerosol-generating substrate can be in the form of a single rod of aerosol-generating substrate. Preferably, the rod of aerosol-generating substrate can include a plurality of thin strips of homogenized dill seed material. Most preferably, the rod of aerosol-generating substrate can include one or more sheets of homogenized dill seed material. Preferably, the one or more sheets of homogenized dill seed material can be crimped such that they have a plurality of ridges or ripples substantially parallel to the cylindrical axis of the rod. This process advantageously facilitates the gathering of the crimped sheets of homogenized dill seed material to form the rod. Preferably, the one or more sheets of homogenized dill seed material can be gathered. It will be appreciated that the crimped sheet of homogenized dill seed material can alternatively or additionally have a plurality of substantially parallel ridges or ripples arranged at acute or obtuse angles to the cylindrical axis of the rod. The sheet can be crimped to such an extent that the integrity of the sheet is disrupted at the plurality of parallel ridges or ripples, causing the material to separate and resulting in the formation of fragments, thin strips, or ribbons of homogenized dill seed material.
[0205] In another embodiment of the aerosol-generating substrate, the homogenized plant material comprises a first rod comprising a first homogenized plant material and a second rod comprising a second homogenized plant material, wherein the first homogenized plant material and the second homogenized plant material comprise different levels of dill seed particles and tobacco particles. For example, the first homogenized plant material may comprise from about 50% to about 75% by weight of dill seed particles on a dry weight basis; while the second homogenized plant material comprises from about 50% to about 75% by weight of tobacco particles on a dry weight basis. In summary, according to the present invention, the homogenized plant material within the aerosol-generating substrate preferably comprises at least 2.5% by weight of dill seed particles and at most 70% by weight of tobacco particles on a dry weight basis.
[0206] In such an arrangement, the first homogenised plant material preferably comprises first particulate plant material having a higher proportion of dill seed particles than the second homogenised plant material.The second homogenised plant material may be a homogenised tobacco material which is substantially free of dill seed particles.
[0207] Preferably, the first homogenised plant material may be in the form of one or more sheets and the second homogenised plant material may be in the form of one or more sheets.
[0208] Optionally, the aerosol-generating substrate may comprise one or more rods. Preferably, the substrate may comprise a first rod and a second rod, wherein the first homogenised plant material may be located in the first rod and the second homogenised plant material may be located in the second rod.
[0209] Two or more rods can be combined and extended in an abutting end-to-end relationship to form a strip. Two rods can be placed longitudinally with a gap between them, thereby creating a cavity within the strip. The rods can be in any suitable arrangement within the strip.
[0210] In another embodiment, the present invention provides a kind of heat conduction sheet material of the present invention.For example, in a preferred arrangement, the downstream rod that comprises the dill seed particles of major proportion can be adjacent to the upstream rod that comprises the tobacco particles of major proportion to form a strip.Also envisioned that wherein the upstream and downstream positions of corresponding rod change relative to each other.Also envisioned that wherein the 3rd homogenized plant material contains the dill seed particles and tobacco particles of different proportions and forms the alternative configuration of the 3rd rod.When two or more rods are provided, the homogenized plant material can be provided in each rod with identical form, or is provided in each rod with different forms, that is, gathers or chopped.Can optionally one or more rods be wrapped in the heat conducting sheet material individually or together as described below.
[0211] The first rod can comprise one or more sheets of the first homogenized plant material, and the second rod can comprise one or more sheets of the second homogenized plant material. The length sum of the rod can be between about 10mm and about 40mm, preferably between about 10mm and about 15mm, more preferably about 12mm. The first rod and the second rod can have the same length or can have different lengths. If the first rod and the second rod have the same length, the length of each rod can preferably be about 6mm to about 20mm. Preferably, the second rod can be longer than the first rod so that the tobacco particles and the dill seed particles of the desired ratio are provided in the matrix. In a word, preferably the matrix contains the tobacco particles of 0 % by weight to 75 % by weight and the dill seed particles of 2.5 % by weight to 75 % by weight on a dry weight basis. Preferably, the second rod is at least 40% to 50% longer than the first rod.
[0212] If the first homogenized plant material and the second homogenized plant material are in the form of one or more sheets, preferably the one or more sheets of the first homogenized plant material and the second homogenized plant material can be aggregated sheets. Preferably, the one or more sheets of the first homogenized plant material and the second homogenized plant material can be press-bonded sheets. It should be understood that all other physical properties described with reference to the embodiment in which a single homogenized plant material is present are equally applicable to the embodiment in which the first homogenized plant material and the second homogenized plant material are present. In addition, it should be understood that the description of additives (such as binders, lipids, fibers, aerosol formers, wetting agents, plasticizers, flavorings, fillers, aqueous and non-aqueous solvents and combinations thereof) with reference to the embodiment in which a single homogenized plant material is present are equally applicable to the embodiment in which the first homogenized plant material and the second homogenized plant material are present.
[0213] In yet another embodiment of the aerosol-generating substrate, the first homogenised plant material is in the form of a first sheet, the second homogenised plant material is in the form of a second sheet, and the second sheet at least partially covers the first sheet.
[0214] The first sheet may be a textured sheet and the second sheet may be non-textured.
[0215] Both the first sheet and the second sheet may be textured sheets.
[0216] The first sheet can be a textured sheet that is textured differently than the second sheet. For example, the first sheet can be crimped while the second sheet can be perforated. Alternatively, the first sheet can be perforated while the second sheet can be crimped.
[0217] The first sheet and the second sheet may both be press-bonded sheets that are different in form from each other. For example, the second sheet may be press-bonded with a different amount of press-bonding per unit width of the sheet than the first sheet.
[0218] These sheets can be gathered to form a rod. The sheets that are gathered together to form a rod can have different physical dimensions. The width and thickness of the sheets can vary.
[0219] It may be necessary to bring together two sheets, each having a different thickness or each having a different width. This may change the physical properties of the rod. This may facilitate blending rods of sheets of different chemical compositions to form an aerosol-generating substrate.
[0220] The first sheet may have a first thickness and the second sheet may have a second thickness, the second thickness being a multiple of the first thickness, for example the second sheet may have a thickness that is twice or three times the first thickness.
[0221] The first sheet may have a first width, and the second sheet may have a second width different from the first width.
[0222] The first sheet and the second sheet may be arranged in an overlapping relationship before being brought together or at the point where they are brought together. The sheets may have the same width and thickness. The sheets may have different thicknesses. The sheets may have different widths. The sheets may have different textures.
[0223] Where it is desired that both the first and second sheets be textured, the sheets may be textured simultaneously prior to being brought together. For example, the sheets may be brought into overlapping relationship and passed through a texturing device, such as a pair of crimping rollers. Figure 2 Suitable apparatus and methods for simultaneous crimping are described. In a preferred embodiment, a second sheet of second homogenized plant material overlays a first sheet of first homogenized plant material, and the combined sheets are gathered to form a rod of aerosol-generating substrate. Optionally, the sheets can be crimped together prior to gathering to facilitate gathering.
[0224] Alternatively, each sheet may be textured separately and then subsequently brought together to form a stick.For example, where the two sheets have different thicknesses, it may be desirable to crimp the first sheet differently relative to the second sheet.
[0225] It will be understood that all other physical properties described with reference to embodiments in which a single homogenized plant material is present are equally applicable to embodiments in which a first homogenized plant material and a second homogenized plant material are present. Furthermore, it will be understood that the description of additives (e.g., binders, lipids, fibers, aerosol formers, humectants, plasticizers, flavorings, fillers, aqueous and non-aqueous solvents, and combinations thereof) with reference to embodiments in which a single homogenized plant material is present are equally applicable to embodiments in which a first homogenized plant material and a second homogenized plant material are present.
[0226] Homogenised plant material for use in an aerosol-generating substrate according to the present invention may be produced by various methods including papermaking, casting, re-agglomeration, extrusion or any other suitable process.
[0227] Preferably, homogenized dill seed material is in the form of " cast leaf ".Term " cast leaf " is used to refer to the sheet product made by cast process in this article, and this process is based on the slurry that will comprise plant particles (for example, the mixture of dill seed particles or tobacco particles and dill seed particles) and binding agent (for example, guar gum) is cast onto a support surface such as on a belt conveyor, makes the slurry dry and takes off the dried sheet from the support surface.For the manufacture of cast leaf tobacco, for example, the example of cast or cast leaf process has been described in US-A-5,724,998.In cast leaf process, granular plant material is mixed with liquid component (normally water), to form slurry.Other added components in the slurry can comprise fiber, binding agent and aerosol forming agent.Particulate plant material can coalesce when there is binding agent.Slurry is cast onto the support surface and dried to form the homogenized dill seed material sheet.
[0228] In certain preferred embodiments, the homogenized dill seed material used in the preparation according to the present invention is produced by casting.The homogenized dill seed material prepared by the casting process generally comprises agglomerated particulate plant material.
[0229] In the cast leaf process, most of the flavoring is advantageously preserved because substantially all of the soluble fraction remains in the plant material. Additionally, the energy-intensive papermaking step is avoided.
[0230] In a preferred embodiment of the present invention, to form the homogenized dill seed material, a mixture comprising particulate plant material, water, a binder, and an aerosol-forming agent is formed. A sheet is formed from the mixture, and the sheet is then dried. Preferably, the mixture is an aqueous mixture. As used herein, "dry weight" refers to the weight of a particular non-aqueous component relative to the total weight of all non-aqueous components in the mixture, expressed as a percentage. The composition of an aqueous mixture can be expressed as "dry weight percentage." This refers to the weight of the non-aqueous component relative to the weight of the entire aqueous mixture, expressed as a percentage.
[0231] The mixture may be a slurry. As used herein, a "slurry" is a homogenised aqueous mixture having a relatively low dry weight. The slurry used in this method preferably has a dry weight of 5% to 60%.
[0232] Alternatively, the mixture may be a mass. As used herein, a "mass" is an aqueous mixture having a relatively high dry weight. The mass used in the methods herein preferably has a dry weight of at least 60%, more preferably at least 70%.
[0233] In certain embodiments of the present methods, it is preferred to comprise greater than 30% slurry and agglomerates by dry weight.
[0234] The step of mixing the particulate plant material, water and other optional components can be carried out by any suitable method. For low viscosity mixtures, i.e., some slurries, it is preferred to use a high energy mixer or a high shear mixer for mixing. This mixing allows the various phases of the mixture to be broken down and evenly distributed. For higher viscosity mixtures, i.e., some lumps, a kneading method can be used to evenly distribute the various phases of the mixture.
[0235] The method according to the present invention may also include a step of vibrating the mixture to distribute the various components. Vibrating the mixture, i.e., vibrating the tank or silo containing the homogenized mixture, for example, can help homogenize the mixture, particularly when the mixture is a low-viscosity mixture, such as some slurries. If vibration is performed as well as mixing, less mixing time may be required to homogenize the mixture to the target value optimal for casting.
[0236] If the mixture is a slurry, a web of homogenized dill seed material is preferably formed by a casting process, which includes casting the slurry onto a supporting surface, such as a belt conveyor. The method for producing the homogenized dill seed material includes the step of drying the cast web to form a sheet. The cast web can be dried at room temperature or at an ambient temperature of at least about 60 degrees Celsius, more preferably at least about 80 degrees Celsius, for an appropriate length of time. Preferably, the cast web is dried at an ambient temperature not exceeding 200 degrees Celsius, more preferably not exceeding about 160 degrees Celsius. For example, the cast web can be dried at a temperature between about 60 degrees Celsius and about 200 degrees Celsius, or between about 80 degrees Celsius and about 160 degrees Celsius. Preferably, the moisture content of the dried sheet is between about 5% and about 15% based on the total weight of the sheet. Then, after drying, the sheet can be removed from the supporting surface. The cast sheet has tensile strength so that it can be mechanically manipulated and wound or unwound from a reel without breaking or deforming.
[0237] If the mixture is in the form of agglomerates, the agglomerates may be extruded in the form of sheets, strips or strips prior to the step of drying the extruded mixture. Preferably, the agglomerates may be extruded in the form of sheets. The extruded mixture may be dried for an appropriate length of time at room temperature or at a temperature of at least about 60 degrees Celsius, more preferably at least about 80 degrees Celsius. Preferably, the extruded mixture is dried at an ambient temperature of no more than 200 degrees Celsius, more preferably no more than about 160 degrees Celsius. For example, the extruded mixture may be dried at a temperature between about 60 degrees Celsius and about 200 degrees Celsius, or between about 80 degrees Celsius and about 160 degrees Celsius. Preferably, the moisture content of the extruded mixture after drying is between about 5% and about 15% based on the gross weight of the sheet. Sheets formed from agglomerates require less drying time and / or a lower drying temperature because the water content is significantly lower relative to webs formed from slurry.
[0238] After the sheet has been dried, the method may optionally comprise the step of applying a nicotine salt, preferably together with an aerosol-forming agent, to the sheet, as described in WO-A-2015 / 082652.
[0239] After the sheet has been dried, the method according to the present invention may optionally include the step of cutting the sheet into strips, fragments, or strips for forming an aerosol-generating substrate as described above. The strips, fragments, or strips may be brought together using suitable means to form a strip of aerosol-generating substrate. In the resulting strip of aerosol-generating substrate, the strips, fragments, or strips may be substantially aligned, for example, in the longitudinal direction of the strip. Alternatively, the strips, fragments, or strips may be randomly oriented within the strip.
[0240] The method according to the invention may optionally further comprise the step of winding the sheet onto a roll after the drying step.
[0241] Alternatively, the homogenized dill seed material can be in the form of dill seed paper. The present invention also provides an alternative papermaking method for producing a sheet of homogenized plant material in the form of plant "paper". Plant paper refers to a reconstituted plant sheet formed by a process in which a plant raw material is extracted with a solvent to produce an extract of soluble plant compounds and an insoluble residue of fibrous plant material, and the extract is recombined with the insoluble residue. Before being recombined with the insoluble residue, the extract may optionally be concentrated or further processed. Before being recombined with the extract, the insoluble residue may optionally be refined and combined with additional plant fiber. In the method according to the present invention, the plant raw material will comprise dill seed particles, optionally in combination with tobacco particles.
[0242] More specifically, the method for producing plant-based paper includes a first step of mixing plant material and water to form a dilute suspension. The dilute suspension primarily comprises individual cellulose fibers. The suspension has a lower viscosity and a higher water content than the slurry produced in the casting process. This first step may include soaking, optionally in the presence of an alkali such as sodium hydroxide, and optionally applying heat.
[0243] The method also includes a second step of separating the suspension into an insoluble fraction containing an insoluble residue of the fibrous plant material and a liquid or aqueous extract containing soluble plant compounds. Water remaining in the insoluble residue of the fibrous plant material can be drained through a screen acting as a sieve, allowing the laydown of a web of randomly interwoven fibers. Water can be further removed from this web by pressing with rollers, sometimes with the assistance of suction or vacuum.
[0244] After removal of the aqueous portion and water, the insoluble residue is formed into a sheet. Preferably, a substantially flat, uniform sheet of plant fiber is formed.
[0245] Preferably, the method further comprises the steps of concentrating an extract of the soluble plant compounds removed from the sheet and adding the concentrated extract to the sheet of insoluble residue of fibrous plant material to form a sheet of homogenized plant material. Alternatively or additionally, soluble plant material or concentrated plant material from another process may be added to the sheet. The extract or concentrated extract may be from another variety of the same plant species or from another plant species.
[0246] This process has been used with tobacco to make reconstituted tobacco products, also known as tobacco paper, as described in US-A-3,860,012. The same method can also be used with one or more plants to produce paper-like sheet materials, such as sheets of dill seed paper.
[0247] In some preferred embodiments, the homogenized plant material used for the products according to the present invention is produced by a papermaking process as defined above. The homogenized tobacco material or the homogenized dill seed material produced by such a process are called tobacco paper or dill seed paper. The homogenized plant material made by papermaking process can be distinguished by a large amount of fibers present in the whole material, and the fiber is visible to the naked eye or visible under an optical microscope, particularly when the paper is wetted with water. By contrast, the homogenized plant material made by the casting process comprises less fiber than paper, and tends to dissociate into slurry when it is wetted. Mixed tobacco dill seed paper refers to the homogenized plant material produced by this method of the mixture using tobacco and dill seed material.
[0248] In embodiments in which the aerosol-generating substrate comprises a combination of dill seed particles and tobacco particles, the aerosol-generating substrate may comprise one or more sheets of dill seed paper and one or more sheets of tobacco paper. The sheets of dill seed paper and tobacco paper may be interlaced or stacked with each other before being gathered to form a strip. Optionally, the sheets may be crimped. Alternatively, the sheets of dill seed paper and tobacco paper may be cut into thin strips, strips, or fragments and then combined to form a strip. The relative amounts of tobacco and dill seed in the aerosol-generating substrate may be adjusted by varying the respective numbers of tobacco and dill seed sheets or the respective amounts of dill seed and tobacco thin strips, strips, or fragments in the strip.
[0249] For example, the number or amount of tobacco and dill seed sheets or strips can be adjusted to provide a dill seed to tobacco ratio of about 1:4, or about 1:9, or about 1:30.
[0250] Other known processes that may be suitable for producing homogenized plant material are agglomerate regeneration processes of the type described, for example, in US-A-3,894,544; and extrusion processes of the type described, for example, in GB-A-983,928. Typically, the density of homogenized plant material produced by extrusion and agglomerate regeneration processes is greater than the density of homogenized plant material produced by casting processes.
[0251] Preferably, the aerosol-generating substrate of an aerosol-generating article according to the present invention comprises at least about 200 mg of homogenised plant material, more preferably at least about 250 mg of homogenised plant material, more preferably at least about 300 mg of homogenised plant material.
[0252] Aerosol-generating articles according to the present invention comprise a strip comprising an aerosol-generating substrate in one or more rods. The strip of aerosol-generating substrate may have a length of about 5 mm to about 120 mm. For example, the strip may preferably have a length of about 10 mm to about 45 mm, more preferably about 10 mm to 15 mm, and most preferably about 12 mm. In alternative embodiments, the strip preferably has a length of about 30 mm to about 45 mm, or about 33 mm to about 41 mm. When the strip is formed from a single rod of aerosol-generating substrate, the rod has the same length as the strip.
[0253] Depending on its intended use, the strip of aerosol-generating substrate may have an outer diameter of about 5 mm to about 10 mm. For example, in some embodiments, the strip may have an outer diameter of about 5.5 mm to about 8 mm, or about 6.5 mm to about 8 mm. The outer diameter of the strip of aerosol-generating substrate corresponds to the diameter of the strip including any packaging.
[0254] The strip of aerosol generating substrate of an aerosol generating article according to the present invention is preferably surrounded along at least a portion of its length by one or more wrappers. The one or more wrappers may comprise a paper wrapper or a non-paper wrapper or both. Suitable paper wrappers for use in particular embodiments of the present invention are known in the art and include, but are not limited to: cigarette paper; and filter segment wrappers. Suitable non-paper wrappers for use in particular embodiments of the present invention are known in the art and include, but are not limited to, sheets of homogenized tobacco material. Homogenized tobacco wrappers are particularly suitable for use in embodiments in which the aerosol generating substrate comprises one or more sheets of homogenized dill seed material formed from a particulate plant material containing a combination of dill seed particles and a low weight percentage of tobacco particles, such as from 20% to 0% by weight of tobacco particles on a dry weight basis.
[0255] In certain embodiments of the present invention, the aerosol-generating substrate is surrounded by a thermally conductive sheet material, for example a metal foil such as aluminium foil or metallized paper, along at least a portion of its length. The metal foil or metallized paper serves the purpose of rapidly conducting heat throughout the aerosol-generating substrate. In addition, the metal foil or metallized paper can be used to prevent ignition of the aerosol-generating substrate in the event that a consumer attempts to ignite it. Furthermore, during use, the metal foil or metallized paper can prevent odours generated when the outer packaging is heated from entering the aerosol generated by the aerosol-generating substrate. For example, this can be a problem for an aerosol-generating article having an aerosol-generating substrate that is heated externally to generate an aerosol during use. Alternatively or additionally, the metallized wrapper can be used to facilitate detection or identification of the aerosol-generating article when the aerosol-generating article is inserted into an aerosol-generating device during use. The metal foil or metallized paper may contain metal particles, such as iron particles.
[0256] The one or more wrappers surrounding the aerosol-generating substrate preferably have a total thickness of from about 0.1 mm to about 0.9 mm.
[0257] The inner diameter of the rod of aerosol-generating substrate is preferably between about 3 mm and about 9.5 mm, more preferably between about 4 mm and about 7.5 mm, and even more preferably between about 5 mm and about 7.5 mm. "Inner diameter" corresponds to the diameter of the rod of aerosol-generating substrate, excluding the thickness of the wrapper, but measured with the wrapper still in place. Aerosol-generating articles according to the present invention also include, but are not limited to, cigarette cartridges or hookah consumables.
[0258] Aerosol-generating articles according to the present invention may optionally include at least one hollow tube immediately downstream of the aerosol-generating substrate. One function of the tube is to position the aerosol-generating substrate toward the distal end of the aerosol-generating article so that it can contact the heating element. When the heating element is inserted into the aerosol-generating substrate, the tube serves to prevent the aerosol-generating substrate from being forced along the aerosol-generating article toward other downstream elements. The tube also serves as a spacer element to separate the downstream elements from the aerosol-generating substrate. The tube can be made of any material, such as cellulose acetate, a polymer, cardboard, or paper.
[0259] The aerosol-generating article according to the present invention optionally includes one or more of a spacer or an aerosol-cooling element downstream of the aerosol-generating substrate and immediately downstream of the hollow tube. In use, an aerosol formed by volatile compounds released from the aerosol-generating substrate passes through the aerosol-cooling element and is cooled by the aerosol-cooling element before being inhaled by the user. The lower temperature allows the vapor to condense into an aerosol. The spacer or aerosol-cooling element can be a hollow tube, such as a hollow cellulose acetate tube or a cardboard tube, which can be similar to the hollow tube immediately downstream of the aerosol-generating substrate. The spacer can be a hollow tube having an outer diameter equal to that of the hollow cellulose acetate tube but an inner diameter smaller or larger than that of the hollow cellulose acetate tube. In one embodiment, the aerosol-cooling element wrapped in paper includes one or more longitudinal channels made of any suitable material, such as metal foil, paper laminated with foil, polymer sheets preferably made of synthetic polymers, and substantially non-porous paper or cardboard. In some embodiments, the aerosol-cooling element wrapped in paper may comprise one or more sheets of a material selected from the group consisting of polyethylene (PE), polypropylene (PP), polyvinyl chloride (PVC), polyethylene terephthalate (PET), polylactic acid (PLA), cellulose acetate (CA), paper laminated with polymer sheets, and aluminum foil. Alternatively, the aerosol-cooling element may be made of woven or non-woven filaments of a material selected from the group consisting of polyethylene (PE), polypropylene (PP), polyvinyl chloride (PVC), polyethylene terephthalate (PET), polylactic acid (PLA), and cellulose acetate (CA). In a preferred embodiment, the aerosol-cooling element is a crimped and gathered sheet of polylactic acid wrapped in filter paper. In another preferred embodiment, the aerosol-cooling element comprises longitudinal channels and is made of woven filaments of a synthetic polymer, such as polylactic acid filaments, wrapped in paper.
[0260] The aerosol-generating article according to the present invention may further comprise a filter or mouthpiece downstream of the aerosol-generating substrate and the hollow cellulose acetate tube, spacer or aerosol-cooling element. The filter may comprise one or more filter materials for removing particulate components, gaseous components or a combination thereof. Suitable filter materials are known in the art and include, but are not limited to: fibrous filter materials such as cellulose acetate tow and paper; adsorbents such as activated alumina, zeolites, molecular sieves and silica gel; biodegradable polymers including, for example, polylactic acid (PLA), Hydrophobic viscose fibers and bioplastics; and combinations thereof. The filter may be located at the downstream end of the aerosol-generating article. The filter may be a cellulose acetate filter segment. In one embodiment, the filter is about 7 mm in length, but may have a length between about 5 mm and about 10 mm.
[0261] Aerosol-generating articles according to the present invention may comprise a mouth-end cavity at the downstream end of the article. The mouth-end cavity may be defined by one or more wrappers extending downstream from the filter or mouthpiece. Alternatively, the mouth-end cavity may be defined by a separate tubular element provided at the downstream end of the aerosol-generating article.
[0262] Aerosol-generating articles according to the invention preferably further comprise a ventilation zone disposed along the aerosol-generating article.For example, the aerosol-generating article may be disposed along a hollow tube disposed downstream of the aerosol-generating substrate.
[0263] In a preferred embodiment of the present invention, the aerosol-generating article comprises an aerosol-generating substrate, at least one hollow tube downstream of the aerosol-generating substrate, and a filter downstream of the at least one hollow tube. Optionally, the aerosol-generating article further comprises a mouth-end cavity at the downstream end of the filter. Preferably, the ventilation zone is provided along the at least one hollow tube.
[0264] In a particularly preferred embodiment of this arrangement, the aerosol-generating substrate has a length of about 33 mm and an outer diameter of about 5.5 mm to 6.7 mm, wherein the aerosol-generating substrate comprises about 340 mg of homogenized dill seed material in the form of a plurality of thin strips, wherein the homogenized dill seed material comprises about 14% glycerol by weight on a dry weight basis. In this embodiment, the aerosol-generating article has a total length of about 74 mm and comprises a cellulose acetate tow filter having a length of about 10 mm and a mouth-end cavity defined by a hollow tube having a length of about 6-7 mm. The aerosol-generating article comprises a hollow tube downstream of the aerosol-generating substrate, wherein the hollow tube has a length of about 25 mm and is provided with a ventilation zone.
[0265] Aerosol-generating articles according to the invention may have an overall length of at least about 30 mm, or at least about 40 mm.The overall length of the aerosol-generating article may be less than 90 mm, or less than about 80 mm.
[0266] In one embodiment, the aerosol-generating article has a total length of about 40 mm to about 50 mm, preferably about 45 mm. In another embodiment, the aerosol-generating article has a total length of about 70 mm to about 90 mm, preferably about 80 mm to about 85 mm. In another embodiment, the aerosol-generating article has a total length of about 72 mm to about 76 mm, preferably about 74 mm.
[0267] The aerosol-generating article may have an outer diameter of about 5 mm to about 8 mm, preferably about 6 mm to about 8 mm. In one embodiment, the aerosol-generating article has an outer diameter of about 7.3 mm.
[0268] Aerosol-generating articles according to the present invention may further comprise one or more aerosol-modifying elements. The aerosol-modifying element may provide an aerosol-modifying agent. As used herein, the term aerosol-modifying agent is used to describe any agent that, during use, modifies one or more characteristics or properties of an aerosol passing through a filter. Suitable aerosol-modifying agents include, but are not limited to, agents that impart a taste or aroma to an aerosol passing through a filter, or agents that remove flavor from an aerosol passing through a filter, during use.
[0269] The aerosol modifier can be one or more of water or liquid flavorings. Water or water can, for example, change the user's sensory experience by wetting the generated aerosol, which can provide a cooling effect to the aerosol and reduce the irritation experienced by the user. The aerosol modifier can be in the form of a flavoring delivery element for delivering one or more liquid flavorings. Alternatively, the liquid flavoring can be added directly to the homogenized plant material, for example, by adding flavorings to a slurry or raw material during the production process of the homogenized plant material, or by spraying the liquid flavoring onto the surface of the homogenized plant material.
[0270] One or more liquid flavorings can comprise any flavoring compound or plant extract, and the flavoring compound or plant extract are suitable for being releasably arranged in the flavoring delivery element in liquid form, to enhance the taste of the aerosol produced during the use of the aerosol-generating article. Liquid or solid flavorings can also be directly arranged in the material forming the filter such as cellulose acetate tow. Suitable flavorings or flavorings include but are not limited to menthol, mint such as peppermint and spearmint, chocolate, liquorice, citrus and other fruit flavors, gamma octalactone, vanillin, ethyl vanillin, breath freshener flavors, spices such as cinnamon, methyl salicylate, linalool, eugenol, bergamot oil, geranium oil, lemon oil and tobacco flavors. Other suitable flavors can include the flavor compounds selected from acid, alcohol, ester, aldehyde, ketone, pyrazine, its combination or blend etc.
[0271] The aerosol modifier may be an adsorbent material such as activated carbon, which removes some of the aerosol constituents that pass through the filter and thereby changes the flavor and aroma of the aerosol.
[0272] One or more aerosol-modifying elements may be located downstream of the aerosol-generating substrate or within the aerosol-generating substrate. The aerosol-generating substrate may include a homogenized dill seed material and an aerosol-modifying element. In various embodiments, the aerosol-modifying element may be placed adjacent to or embedded in the homogenized dill seed material. Typically, the aerosol-modifying element may be located downstream of the aerosol-generating substrate, most typically within an aerosol-cooling element, within a filter of an aerosol-generating article, such as within a filter segment or within a cavity between filter segments. The one or more aerosol-modifying elements may be in the form of one or more of a thread, capsule, microcapsule, bead, or polymer-based material, or a combination thereof.
[0273] If the aerosol modifying element is in the form of a thread, as described in WO-A-2011 / 060961, the thread may be formed from paper such as a filter segment wrapper, and the thread may be loaded with at least one aerosol modifying agent and located within the filter body. Other materials that may be used to form the thread include cellulose acetate and cotton.
[0274] If the aerosol modifying element is in the form of a capsule, as described in WO-A-2007 / 010407, WO-A-2013 / 068100, and WO-A-2014 / 154887, the capsule can be a breakable capsule positioned within the filter, with the inner core of the capsule containing the aerosol modifying agent, which can be released when the outer shell of the capsule is broken when the filter is subjected to an external force. The capsule can be positioned within the filter segment or within the cavity between filter segments.
[0275] If the aerosol modifying element is the form of polymer matrix material, then when heating aerosol generates goods, for example when heating polymer matrix exceeds the fusing point of polymer matrix material, polymer matrix material releases flavoring, as described in WO-A-2013 / 034488.Usually, this polymer matrix material can be positioned in the beads in the aerosol generation matrix.Alternatively or additionally, flavoring can be trapped in the territory of polymer matrix material, and can discharge from polymer matrix material when compressing polymer matrix material.Preferably, flavoring is discharged when compressing polymer matrix material with about 15 Newton's power.This type of flavor improving component can be within the power range of at least 5 Newtons, such as between 5N and 20N, the sustained release of liquid flavoring is provided, as described in WO2013 / 068304.Usually, such polymer matrix material can be positioned in the beads in the filter.
[0276] The aerosol-generating article may comprise a combustible heat source and an aerosol-generating substrate downstream of the combustible heat source, the aerosol-generating substrate being as described above in relation to the first aspect of the invention.
[0277] For example, a substrate as described herein may be used in a heated aerosol-generating article of the type disclosed in WO-A-2009 / 022232, comprising a combustible carbon-based heat source, an aerosol-generating substrate downstream of the combustible heat source, and a heat-conductive element surrounding and in contact with a rear portion of the combustible carbon-based heat source and an adjacent front portion of the aerosol-generating substrate. However, it will be understood that a substrate as described herein may also be used in heated aerosol-generating articles comprising combustible heat sources having other configurations.
[0278] The present invention provides an aerosol-generating system comprising an aerosol-generating device comprising a heating element, and an aerosol-generating article for use with the aerosol-generating device, the aerosol-generating article comprising an aerosol-generating substrate as described above.
[0279] In a preferred embodiment, an aerosol-generating substrate as described herein may be used in a heated aerosol-generating article for use in an electrically operated aerosol-generating system, wherein the aerosol-generating substrate of the heated aerosol-generating article is heated by an electric heat source.
[0280] For example, an aerosol-generating substrate as described herein may be used in a heated aerosol-generating article of the type disclosed in EP-A-0 822 760.
[0281] The heating element of such an aerosol-generating device may be of any suitable form for conducting heat. Heating of the aerosol-generating substrate may be achieved internally, externally, or both internally and externally. The heating element may preferably be a heater blade or pin adapted to be inserted into the substrate so that the substrate is heated from the inside. Alternatively, the heating element may partially or completely surround the substrate and heat the substrate circumferentially from the outside.
[0282] The aerosol-generating system may be an electrically operated aerosol-generating system that includes an induction heating device. The induction heating device typically comprises an induction source configured to couple to a susceptor, which may be disposed externally to or internally within the aerosol-generating substrate. The induction source generates an alternating electromagnetic field that induces magnetization or eddy currents in the susceptor. The susceptor may be heated due to hysteresis losses or induced eddy currents, which heat the susceptor via ohmic or resistive heating.
[0283] An electrically operated aerosol-generating system comprising an induction heating device may further comprise an aerosol-generating article comprising an aerosol-generating substrate and a susceptor in thermal proximity to the aerosol-generating substrate. Typically, the susceptor is in direct contact with the aerosol-generating substrate, and heat is transferred from the susceptor to the aerosol-generating substrate primarily by conduction. Examples of electrically operated aerosol-generating systems comprising an induction heating device and aerosol-generating articles comprising a susceptor are described in WO-A1-95 / 27411 and WO-A1-2015 / 177255.
[0284] The susceptor can be a plurality of susceptor particles that can be deposited on or embedded in the aerosol-generating matrix. When the aerosol-generating matrix is in the form of one or more sheets, a plurality of susceptor particles can be deposited on or embedded in the one or more sheets. The susceptor particles are fixed by a matrix, for example in the form of a sheet, and are maintained in an initial position. Preferably, the susceptor particles can be evenly distributed in the homogenized dill seed material of the aerosol-generating matrix. Due to the particulate nature of the susceptors, heat is generated according to the distribution of the particles in the homogenized dill seed material sheet of the matrix. Alternatively, one or more susceptors in the form of sheets, strips, fragments or strips can be placed next to the homogenized dill seed material or used in the form of being embedded in the homogenized dill seed material. In one embodiment, the aerosol-forming matrix comprises one or more susceptor strips. In another embodiment, the susceptor is present in the aerosol-generating device.
[0285] The susceptor may have a heat loss of greater than 0.05 joules / kg, preferably greater than 0.1 joules / kg. Heat loss is the ability of the susceptor to transfer heat to the surrounding material. Because the susceptor particles are preferably uniformly distributed in the aerosol-generating substrate, a uniform heat loss from the susceptor particles can be achieved, thereby generating a uniform heat distribution in the aerosol-generating substrate and resulting in a uniform temperature distribution in the aerosol-generating article. It has been found that a specific minimum heat loss of 0.05 joules / kg in the susceptor particles allows the aerosol-generating substrate to be heated to a substantially uniform temperature, thereby providing aerosol generation. Preferably, in such embodiments, the average temperature achieved within the aerosol-generating substrate is about 200 degrees Celsius to about 240 degrees Celsius.
[0286] Reducing the risk of overheating the aerosol-generating substrate can be aided by using a susceptor material with a Curie temperature, which allows heating to proceed only up to a certain maximum temperature due to hysteresis losses. The susceptor can have a Curie temperature between approximately 200°C and approximately 450°C, preferably between approximately 240°C and approximately 400°C, for example, approximately 280°C. When the susceptor material reaches its Curie temperature, its magnetic properties change. At the Curie temperature, the susceptor material changes from a ferromagnetic phase to a paramagnetic phase. At this point, heating based on energy loss ceases due to the alignment of the ferromagnetic domains. In addition, heating is primarily based on eddy current formation, so that the heating process automatically subsides when the Curie temperature of the susceptor material is reached. Preferably, the susceptor material and its Curie temperature are adapted to the composition of the aerosol-generating substrate to achieve an optimal temperature and temperature distribution within the aerosol-generating substrate for optimal aerosol generation.
[0287] In some preferred embodiments of the aerosol generating article according to the present invention, the susceptor is made of ferrite. Ferrite is a ferromagnetic material with high magnetic permeability and is particularly suitable as a susceptor material. The main component of ferrite is iron. Other metal components, such as zinc, nickel, manganese or non-metallic components such as silicon, may be present in different amounts. Ferrite is a relatively cheap commercially available material. Ferrite can be obtained in the form of particles with a size range that is the size range of the particles in the granular plant material used to form the homogenized plant material according to the present invention. Preferably, the particles are fully sintered ferrite powder, such as FP160, FP215, FP350 produced by PPT in Indiana, USA.
[0288] In certain embodiments of the present invention, the aerosol generating system comprises an aerosol generating article, the aerosol generating article comprising an aerosol generating substrate as defined above, an aerosol forming agent source and a device for evaporating the aerosol forming agent, preferably a heating element as described above. The aerosol forming agent source can be a refillable or replaceable reservoir located on the aerosol generating device. When the reservoir is physically separated from the aerosol generating article, the generated vapor is directed through the aerosol generating article. The vapor contacts the aerosol generating substrate, which releases volatile compounds, such as nicotine and flavorings in the particulate plant material, to form an aerosol. Optionally, in order to assist in the volatilization of the compounds in the aerosol generating substrate, the aerosol generating system may also comprise a heating element to heat the aerosol generating substrate, preferably in a manner coordinated with the aerosol forming agent. However, in certain embodiments, the heating element for heating the aerosol generating article is separate from the heater that heats the aerosol forming agent.
[0289] The present invention also provides an aerosol generated upon heating an aerosol-forming substrate as defined above, wherein the aerosol comprises the characteristic compounds derived from dill seed particles in the specific amounts and ratios as defined above.
[0290] According to the present invention, the aerosol comprises: carvone in an amount of at least 0.5 micrograms per puff of the aerosol; and limonene in an amount of at least 0.05 micrograms per puff of the aerosol, wherein one puff of the aerosol has a volume of 55 milliliters as generated by a smoking machine. For the purposes of the present invention, a "puff" is defined as the volume of aerosol released from an aerosol-generating substrate upon heating and collected for analysis, wherein a puff of the aerosol, as generated by a smoking machine, has a puff volume of 55 milliliters. Therefore, unless otherwise specified, any reference herein to a "puff" of an aerosol should be understood to refer to a 55 milliliter puff.
[0291] The indicated ranges define the total amount of each component measured in a 55 ml puff of aerosol. The aerosol can be generated from an aerosol-generating substrate using any suitable device and can be captured and analyzed as described above to identify characteristic compounds within the aerosol and measure their amounts. For example, a "puff" can correspond to a 55 ml puff taken on a smoking machine, such as the puff used in the Health Canada test method described herein.
[0292] Preferably, the aerosol according to the present invention comprises at least about 2 micrograms of carvone per puff of aerosol, more preferably at least about 5 micrograms of carvone per puff of aerosol. Alternatively or additionally, the aerosol generated by the aerosol-generating substrate comprises at most about 50 micrograms of carvone per puff of aerosol, preferably at most about 40 micrograms of carvone per puff of aerosol, more preferably at most about 25 micrograms of carvone per puff of aerosol. For example, the aerosol generated by the aerosol-generating substrate may comprise from about 0.1 micrograms to about 50 micrograms of carvone per puff of aerosol, or from about 2 micrograms of carvone per puff of aerosol to about 40 micrograms of carvone per puff of aerosol, or from about 5 micrograms to about 25 micrograms of carvone per puff of aerosol.
[0293] Preferably, the aerosol according to the present invention comprises at least about 0.2 μg of limonene per puff of aerosol, more preferably at least about 0.5 μg of limonene per puff of aerosol. Alternatively or additionally, the aerosol generated by the aerosol-generating substrate preferably comprises at most about 10 μg of limonene per puff of aerosol, more preferably at most about 8 μg of limonene per puff of aerosol, and even more preferably at most about 6 μg of limonene per puff of aerosol. For example, the aerosol generated by the aerosol-generating substrate may comprise from about 0.05 μg to about 10 μg of limonene per puff of aerosol, or from about 0.2 μg to about 8 μg of limonene per puff of aerosol, or from about 0.5 μg to about 6 μg of limonene per puff of aerosol.
[0294] According to the present invention, the aerosol composition is such that the amount of carvone per puff of the aerosol is preferably no more than about 10 times the amount of limonene per puff of the aerosol. Thus, the ratio of carvone to limonene in the aerosol is preferably no more than about 10:1. Preferably, the aerosol composition is such that the amount of carvone per puff of the aerosol is no more than about 8 times the amount of limonene per puff of the aerosol.
[0295] Said defined ratio of carvone to limonene characterizes an aerosol originating from dill seed particles. In contrast, in an aerosol generated from dill essential oil, the ratio of carvone to limonene will be significantly different.
[0296] Preferably, the aerosol according to the present invention further comprises at least about 0.1 mg of aerosol former per puff, more preferably at least about 0.2 mg of aerosol per puff, more preferably at least about 0.3 mg of aerosol former per puff. Preferably, the aerosol comprises at most 0.6 mg of aerosol former per puff, more preferably at most 0.5 mg of aerosol former per puff, more preferably at most 0.4 mg of aerosol former per puff. For example, the aerosol may comprise from about 0.1 mg to about 0.6 mg of aerosol former per puff, or from about 0.2 mg to about 0.5 mg of aerosol former per puff, or from about 0.3 mg to about 0.4 mg of aerosol former per puff. These values are based on a puff volume of 55 ml as defined above.
[0297] Suitable aerosol formers for use in the present invention are described above.
[0298] Preferably, the aerosol generated by the aerosol-generating substrate according to the present invention also comprises at least about 2 micrograms of nicotine per puff of aerosol, more preferably at least about 20 micrograms of nicotine per puff of aerosol, more preferably at least about 40 micrograms of nicotine per puff of aerosol. Preferably, the aerosol comprises at most about 200 micrograms of nicotine per puff of aerosol, more preferably at most about 150 micrograms of nicotine per puff of aerosol, more preferably at most about 75 micrograms of nicotine per puff of aerosol. For example, the aerosol may comprise from about 2 micrograms to about 200 micrograms of nicotine per puff of aerosol, or from about 20 micrograms to about 150 micrograms of nicotine per puff of aerosol, or from about 40 micrograms to about 75 micrograms of nicotine per puff of aerosol. These values are based on a puff volume of 55 milliliters as defined above. In some embodiments of the present invention, the aerosol may contain zero micrograms of nicotine.
[0299] Carbon monoxide may also be present in aerosols according to the present invention and may be measured and used to further characterize the aerosol.Nitrogen oxides such as nitric oxide and nitrogen dioxide may also be present in aerosols and may be measured and used to further characterize the aerosol.
[0300] Aerosols according to the present invention comprising characteristic compounds from dill seed particles can be formed from particles having a mass median aerodynamic diameter (MMAD) in the range of about 0.01 to 200 microns or about 1 to 100 microns. Preferably, when the aerosol comprises nicotine as described above, the aerosol comprises particles having an MMAD in the range of about 0.1 to about 3 microns to optimize the delivery of nicotine from the aerosol.
[0301] The mass median aerodynamic diameter (MMAD) of an aerosol is the aerodynamic diameter at which half of the aerosol's mass is contributed by particles with aerodynamic diameters greater than the MMAD and half by particles with aerodynamic diameters less than the MMAD. The aerodynamic diameter is defined as the mass median aerodynamic diameter of an aerosol with a density of 1 g / cm 3 The diameter of a spherical particle that has the same settling velocity as the characterized particle.
[0302] The mass median aerodynamic diameter of the aerosol according to the present invention can be determined according to Section 2.8 of Schaller et al., “Evaluation of the Tobacco Heating System 2.2. Part 2: Chemical composition, genotoxicity, cytotoxicity and physical properties of the aerosol,” Regul. Toxicol. and Pharmacol., 81 (2016) S27-S47.
[0303] The present invention also provides an aerosol-generating article comprising an aerosol-generating substrate, as defined above, said aerosol-generating substrate comprising homogenised plant material, wherein upon heating said aerosol-generating substrate according to Test Method A, said aerosol generated from said aerosol-generating substrate comprises: carvone in an amount of at least 0.5 micrograms per puff aerosol; and limonene in an amount of at least 0.05 micrograms per puff aerosol, wherein the amount of carvone per puff aerosol is no more than about 10 times the amount of limonene per puff aerosol and wherein one puff aerosol has a volume of 55 millilitres as generated by a smoking machine.
[0304] For the purposes of the present invention, a "puff" is defined as the volume of aerosol released from an aerosol-generating substrate upon heating and collected for analysis, wherein the puff of the aerosol has a puff volume of 55 ml, as generated by a smoking machine. Therefore, unless otherwise indicated, any reference herein to a "puff" of an aerosol should be understood to refer to a 55 ml puff. The indicated ranges define the total amount of each component measured in a 55 ml puff of the aerosol. The aerosol can be generated from the aerosol-generating substrate using any suitable device and can be captured and analyzed as described above in order to identify characteristic compounds within the aerosol and measure their amounts. For example, a "puff" may correspond to a 55 ml puff taken on a smoking machine, such as the puff used in the Health Canada test method described herein.
[0305] The present invention also provides an aerosol-generating substrate formed from homogenised plant material, as defined above, comprising at least about 2.5% by weight on a dry weight basis of dill seed particles, an aerosol-former and a binder, wherein the aerosol-generating substrate comprises: at least 100 micrograms of carvone per gram of substrate on a dry weight basis; and at least 2 micrograms of limonene per gram of substrate on a dry weight basis, wherein the amount of carvone per gram of substrate is no more than about 50 times the amount of limonene per gram of substrate.
[0306] A non-exhaustive list of non-limiting examples is provided below.Any one or more features of these examples may be combined with any one or more features of another example, embodiment or aspect described herein.
[0307] EX1. An aerosol-generating article comprising an aerosol-generating substrate, the aerosol-generating substrate comprising a homogenized dill seed material, the homogenized dill seed material comprising dill seed particles, an aerosol-forming agent, and a binder, wherein the aerosol-generating substrate comprises:
[0308] at least 100 micrograms of carvone per gram of said substrate on a dry weight basis; and
[0309] At least 2 micrograms of limonene per gram of said substrate on a dry weight basis.
[0310] EX2. An aerosol-generating article according to example EX1, wherein the amount of carvone per gram of substrate is no more than 50 times the amount of limonene per gram of substrate.
[0311] EX3. An aerosol-generating article according to example EX1 or EX2, wherein the aerosol-generating substrate comprises from 100 μg to 4500 μg of carvone per gram of substrate on a dry weight basis.
[0312] EX4. The aerosol-generating article according to any one of examples EX1 to EX3, wherein the aerosol-generating substrate comprises 2 to 200 micrograms of limonene per gram of substrate on a dry weight basis.
[0313] EX5. An aerosol-generating article according to any one of Examples EX1 to EX4, wherein upon heating the aerosol-generating substrate according to Test Method A, the generated aerosol comprises:
[0314] at least 20 micrograms of carvone per gram of said substrate on a dry weight basis; and
[0315] at least 2 micrograms of limonene per gram of said substrate on a dry weight basis,
[0316] The amount of carvone in the aerosol per gram of the substrate is not more than 10 times the amount of limonene in the aerosol per gram of the substrate.
[0317] EX6. An aerosol-generating article according to example EX5, wherein upon heating the aerosol-generating substrate according to Test Method A, the generated aerosol comprises at most 1500 micrograms of carvone per gram of substrate on a dry weight basis.
[0318] EX7. An aerosol-generating article according to example EX5 or EX6, wherein upon heating the aerosol-generating substrate according to Test Method A, the generated aerosol comprises at most 300 micrograms of limonene per gram of substrate on a dry weight basis.
[0319] EX8. The aerosol-generating article of any one of examples EX5 to EX7, wherein upon heating the aerosol-generating substrate according to Test Method A, the generated aerosol comprises zero micrograms of nicotine per gram of substrate.
[0320] EX9. An aerosol-generating article according to any one of Examples EX1 to EX4, wherein upon heating the aerosol-generating substrate in a THS2.2 holder according to the Health Canada machine smoking protocol, the generated aerosol comprises:
[0321] at least 20 micrograms of carvone per gram of said substrate on a dry weight basis; and
[0322] at least 2 micrograms of limonene per gram of said substrate on a dry weight basis,
[0323] The amount of carvone in the aerosol per gram of the substrate is not more than 10 times the amount of limonene in the aerosol per gram of the substrate.
[0324] EX10. The aerosol-generating article according to any one of examples EX1 to EX9, wherein the homogenized dill seed material comprises at least 2.5 wt% dill seed particles on a dry weight basis.
[0325] EX11. The aerosol-generating article according to any one of examples EX1 to EX10, wherein the homogenized dill seed material comprises at most 25 wt% dill seed particles on a dry weight basis.
[0326] EX12. The aerosol-generating article according to any one of examples EX1 to EX11, wherein the homogenized dill seed material comprises at most 65 wt% dill seed particles on a dry weight basis.
[0327] EX13. The aerosol-generating article according to any one of examples EX1 to EX12, wherein the homogenized dill seed material further comprises up to about 75 wt% tobacco particles on a dry weight basis.
[0328] EX14. The aerosol-generating article according to any one of examples EX1 to EX13, wherein the homogenized dill seed material further comprises tobacco particles and wherein the weight ratio of dill seed particles to tobacco particles is no greater than 1:4.
[0329] EX15. The aerosol-generating article according to example EX13 or EX14, wherein the homogenized dill seed material comprises 5 wt% to 20 wt% dill seed particles and 55 wt% to 70 wt% tobacco particles on a dry weight basis.
[0330] EX16. The aerosol-generating article according to any one of examples EX1 to EX15, wherein the homogenized dill seed material comprises essentially zero nicotine.
[0331] EX17. The aerosol-generating article according to any one of examples EX1 to EX15, wherein the aerosol-generating substrate further comprises at least 0.1 mg nicotine per gram of substrate by dry weight.
[0332] EX18. The aerosol-generating article according to example EX17, wherein the aerosol-generating substrate comprises from 1 mg to 20 mg of nicotine per gram of substrate by dry weight.
[0333] EX19. The aerosol-generating article according to any one of examples EX1 to EX18, wherein the dill seed particles have a D95 value of greater than or equal to about 200 microns to a D95 value of less than or equal to about 900 microns.
[0334] EX20. The aerosol-generating article according to any one of examples EX1 to EX19, wherein the dill seed particles have a D5 value of greater than or equal to about 10 microns to a D5 value of less than or equal to about 50 microns.
[0335] EX21. The aerosol-generating article according to any one of examples EX1 to EX20, wherein the dill seed particles are purposefully ground.
[0336] EX22. The aerosol-generating article according to any one of examples EX1 to EX21, wherein 100% of the dill seed particles have a diameter less than or equal to 300 microns.
[0337] EX23. The aerosol-generating article according to any one of examples EX1 to EX22, wherein the homogenized dill seed material comprises up to 75% by weight of the particulate plant material, the particulate plant material comprising dill seed particles.
[0338] EX24. The aerosol-generating article according to any one of examples EX1 to EX23, wherein the homogenized dill seed material has an aerosol-former content of 5 wt% to 30 wt% on a dry weight basis.
[0339] EX25. An aerosol-generating article according to any one of Examples EX1 to EX24, wherein the binder is selected from: gums such as guar gum, xanthan gum, gum arabic and locust bean gum; cellulosic binders such as hydroxypropyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, methyl cellulose and ethyl cellulose; polysaccharides such as starch; organic acids such as alginic acid; conjugate base salts of organic acids such as sodium alginate; agar and pectin; and combinations thereof.
[0340] EX26. The aerosol-generating article according to any one of examples EX1 to EX25, wherein the homogenized dill seed material comprises 1 wt% to 10 wt% of the binder on a dry weight basis.
[0341] EX27. The aerosol-generating article according to any one of examples EX1 to EX26, wherein the binder comprises guar gum.
[0342] EX28. The aerosol-generating article according to any one of examples EX1 to EX26, wherein the binder comprises a cellulose ether and wherein the homogenized dill seed material comprises from about 2 wt% to about 10 wt% of the cellulose ether.
[0343] EX29. The aerosol-generating article of example EX28, wherein the homogenized dill material further comprises additional cellulose not derived from dill seed particles, wherein the additional cellulose comprises at least one of cellulose powder and cellulose fibers.
[0344] EX30. The aerosol-generating article according to example EX29, wherein the ratio of additional cellulosic material to cellulose ether in the homogenized dill seed material is at least 2.
[0345] EX31. An aerosol-generating article according to EX29 or EX30, wherein the homogenized dill material comprises: 2.5 wt% to 75 wt% dill seed particles on a dry weight basis; 15 wt% to 55 wt% aerosol-forming agent on a dry weight basis; 2 wt% to 10 wt% cellulose ether on a dry weight basis; and 3 wt% to 50 wt% additional cellulose on a dry weight basis.
[0346] EX32. The aerosol-generating article according to any one of examples EX1 to EX31, wherein the homogenized dill seed material further comprises fiber.
[0347] EX33. An aerosol-generating article according to example EX32, wherein the fibers have a length greater than 400 microns.
[0348] EX34. The aerosol-generating article according to example EX32 or EX33, wherein the fibers are present in an amount from about 2 wt% to about 15 wt% based on the dry weight of the aerosol-generating substrate.
[0349] EX35. The aerosol-generating article according to example EX32 or EX33, wherein the fibers are present in an amount of at least 30 wt.-%, based on the dry weight of the aerosol-generating substrate.
[0350] EX36. The aerosol-generating article of any one of examples EX1 to EX35, wherein the homogenized dill seed material comprises dill seed particles, about 5 wt% to about 30 wt% aerosol-former, and about 1 wt% to about 10 wt% binder on a dry weight basis.
[0351] EX37. The aerosol-generating article of example EX36, wherein the homogenized dill seed material further comprises from about 2 wt% to about 15 wt% fiber.
[0352] EX38. An aerosol-generating article according to example EX36 or EX37, wherein the binder is guar gum.
[0353] EX39. The aerosol-generating article according to any one of examples EX1 to EX38, wherein the homogenized dill seed material is in the form of one or more sheets.
[0354] EX40. The aerosol-generating article of example EX39, wherein each of the one or more sheets has a thickness of 100 to 600 micrometers.
[0355] EX41. An aerosol-generating article according to example EX39, wherein each of the one or more sheets has a viscosity of 100 g / m 2 Up to 300g / m 2 Gram weight per square meter.
[0356] EX42. An aerosol-generating article according to any one of Examples EX39 to EX41, wherein each of the one or more sheets has a viscosity of 0.3 g / cm 3 to 1.3g / cm 3 density.
[0357] EX43. The aerosol-generating article according to any of examples EX39 to EX42, wherein each of the one or more sheets has a transverse direction peak tensile strength of 50 N / m to 400 N / m.
[0358] EX44. The aerosol-generating article according to any of examples EX39 to EX43, wherein each of the one or more sheets has a longitudinal peak tensile strength of 100 N / m to 800 N / m.
[0359] EX45. The aerosol-generating article according to any one of examples EX39 to EX44, wherein the one or more sheets are in the form of one or more gathered sheets.
[0360] EX46. An aerosol-generating article according to any one of examples EX1 to EX38, wherein the homogenized dill seed material is in the form of a plurality of thin strips.
[0361] EX47. An aerosol-generating article according to example EX46, wherein the width of the strips is at least 0.2 mm.
[0362] EX48. An aerosol-generating article according to example EX46 or EX47, wherein the plurality of strips extend substantially longitudinally along the length of the aerosol-generating substrate aligned with the longitudinal axis.
[0363] EX49. An aerosol-generating article according to example EX46, EX47 or EX48, wherein each of the plurality of strips has a mass-to-surface-area ratio of at least 0.02 mg / mm2.
[0364] EX50. The aerosol-generating article according to any one of examples EX1 to EX49, wherein the homogenized dill seed material in the aerosol-generating substrate is in the form of cast leaves.
[0365] EX51. The aerosol-generating article according to any one of examples EX1 to EX49, wherein the homogenized dill seed material in the aerosol-generating substrate is in the form of dill seed paper.
[0366] EX52. An aerosol-generating article according to any one of Examples EX1 to EX51, wherein upon heating the aerosol-generating substrate according to Test Method A, the aerosol generated by the aerosol-generating substrate comprises:
[0367] Carvone in an amount of at least 0.5 micrograms per aerosol puff; and
[0368] At least 0.05 micrograms of limonene per aerosol puff,
[0369] wherein the aerosol per puff has a volume of 55 ml as generated by a smoking machine, and wherein the amount of carvone per puff aerosol is no more than 10 times the amount of limonene per puff aerosol.
[0370] EX53. An aerosol-generating article comprising an aerosol-generating substrate, the aerosol-generating substrate comprising a homogenized dill seed material, the homogenized dill seed material comprising dill seed particles, from about 5 wt% to about 30 wt% of an aerosol former and from about 1 wt% to about 10 wt% of a binder on a dry weight basis.
[0371] EX54. An aerosol-generating article according to example EX53, wherein the homogenized dill seed material further comprises an essential oil, preferably dill seed essential oil.
[0372] EX55. An aerosol-generating article according to example EX53 or EX54, wherein the homogenized dill seed material further comprises tobacco particles.
[0373] EX56. The aerosol-generating article according to any one of examples EX53 to EX55, wherein the homogenized dill seed material comprises at least 2.5 wt% dill seed particles on a dry weight basis.
[0374] EX57. An aerosol-generating substrate comprising a homogenized dill seed material comprising dill seed particles, an aerosol-forming agent, and a binder, wherein the aerosol-generating substrate comprises:
[0375] At least 100 μg carvone / g substrate on a dry weight basis;
[0376] At least 2 micrograms of limonene per gram of substrate on a dry weight basis, wherein the amount of carvone per gram of substrate is not more than 50 times the amount of limonene per gram of substrate.
[0377] EX58. An aerosol generating system, comprising:
[0378] an aerosol generating device comprising a heating element; and
[0379] An aerosol-generating article according to any of Examples EX1 to EX56.
[0380] EX59. An aerosol-generating system according to example EX58, wherein the heating element is a heater blade adapted to be inserted into the aerosol-generating substrate.
[0381] EX60. An aerosol generated upon heating the aerosol-generating substrate according to example EX57, the aerosol comprising:
[0382] Carvone in an amount of at least 0.5 micrograms per aerosol puff; and
[0383] At least 0.05 micrograms of limonene per aerosol puff,
[0384] wherein the one-puff aerosol has a volume of 55 ml as generated by a smoking machine and wherein the amount of carvone per gram of substrate is no more than 10 times the amount of carvone per gram of substrate.
[0385] EX61. A method of manufacturing an aerosol-generating substrate, the method comprising the steps of:
[0386] forming a slurry comprising dill seed particles, water, an aerosol former, a binder, and optionally tobacco particles;
[0387] Casting or extruding the slurry into a sheet or strip form; and
[0388] The sheets or strips are dried at 80 to 160 degrees Celsius.
[0389] EX62. The method of example EX60, wherein the slurry is cast onto a support surface and dried to form a sheet of cast leaves.
[0390] EX63. A method of manufacturing an aerosol-generating substrate, the method comprising the steps of:
[0391] forming a dilute suspension comprising dill seed particles, water, and optionally tobacco particles;
[0392] separating the suspension into an insoluble portion and a liquid extract;
[0393] forming the insoluble portion into a sheet;
[0394] The liquid extract is concentrated and the concentrated liquid extract is added to a sheet material to form dill seed paper.
[0395] Certain embodiments will be further described, by way of example only, with reference to the accompanying drawings, in which:
[0396] Figure 1 A first embodiment of a substrate for an aerosol-generating article as described herein is shown;
[0397] Figure 2 An aerosol-generating system comprising an aerosol-generating article and an aerosol-generating device comprising an electric heating element is shown;
[0398] Figure 3 An aerosol-generating system comprising an aerosol-generating article and an aerosol-generating device including a combustible heating element is shown;
[0399] Figure 4a and 4b A second embodiment of a substrate for an aerosol-generating article as described herein is shown;
[0400] Figure 5 A third embodiment of a substrate for an aerosol-generating article as described herein is shown;
[0401] Figure 6a 、 6b 6c each show a cross-sectional view of a filter 1050 further comprising an aerosol modifying element, wherein
[0402] Figure 6a An aerosol-modifying element in the form of spherical capsules or beads within a filter segment is shown.
[0403] Figure 6b An aerosol-modifying element is shown in the form of a thread within a filter segment.
[0404] Figure 6c An aerosol-modifying element in the form of a spherical capsule within a cavity within the filter is shown;
[0405] Figure 7 is a cross-sectional view of a rod of an aerosol-generating substrate 1020 additionally comprising an elongate susceptor element; and
[0406] Figure 8 Shown is the experimental setup for collecting aerosol samples to be analyzed for the measurement of characteristic compounds.
[0407] Figure 1 A heated aerosol-generating article 1000 comprising a substrate as described herein is illustrated. The article 1000 comprises four elements: an aerosol-generating substrate 1020, a hollow cellulose acetate tube 1030, a spacer element 1040, and a mouthpiece filter 1050. These four elements are arranged sequentially and in coaxial alignment and assembled by rolling paper 1060 to form the aerosol-generating article 1000. The article 1000 has an oral end 1012 that a user inserts into his or her mouth during use, and a distal end 1013 located at the end of the article opposite the oral end 1012. Figure 1 The embodiment of the aerosol-generating article illustrated in is particularly suitable for use with an electrically operated aerosol-generating device comprising a heater for heating the aerosol-generating substrate.
[0408] When assembled, the article 1000 is approximately 45 mm in length and has an outer diameter of approximately 7.2 mm and an inner diameter of approximately 6.9 mm.
[0409] The aerosol-generating substrate 1020 comprises a rod formed from a sheet of homogenised dill seed material containing dill seed particles alone or in combination with tobacco particles.
[0410] Table 1 below shows several examples of suitable homogenized dill seed materials (see samples B to D) for forming the aerosol-generating substrate 1020. The sheets were gathered, crimped, and wrapped in filter paper (not shown) to form a stick. The sheets contained additives, including glycerol as an aerosol former.
[0411] like Figure 1 The aerosol-generating article 1000 shown in FIG is designed to be engaged with an aerosol-generating device for consumption. Such an aerosol-generating device includes means for heating the aerosol-generating substrate 1020 to a sufficient temperature to form an aerosol. Typically, the aerosol-generating device may include a heating element surrounding the aerosol-generating article 1000 adjacent to the aerosol-generating substrate 1020, or a heating element inserted into the aerosol-generating substrate 1020.
[0412] Once engaged with the aerosol-generating device, the user draws on the mouth end 1012 of the smoking article 1000, and the aerosol-generating substrate 1020 is heated to a temperature of approximately 375 degrees Celsius. At this temperature, volatile compounds are emitted from the aerosol-generating substrate 1020. These compounds condense to form an aerosol. The aerosol is drawn through the filter 1050 and into the user's mouth.
[0413] Figure 2 A portion of an electrically operated aerosol generating system 2000 is shown which utilizes a heating blade 2100 to heat the aerosol generating substrate 1020 of an aerosol generating article 1000. The heating blade is mounted within an aerosol article receiving chamber of an electrically operated aerosol generating device 2010. The aerosol generating device defines a plurality of air holes 2050 to allow air to flow to the aerosol generating article 1000. The air flow is controlled by Figure 2 The aerosol generating device includes a power source and electronic components, which are not in the Figure 2 Shown in. Figure 2 The aerosol generating article 1000 is as follows Figure 1 described.
[0414] exist Figure 3 In the alternative configuration shown in , the aerosol generating system is shown having a combustible heating element. Figure 1 The article 1000 is intended to be consumed in conjunction with an aerosol generating device, but Figure 3 The article 1001 of the invention comprises a combustible heat source 1080 which can be ignited and transfers heat to the aerosol-generating substrate 1020 to form an inhalable aerosol. The combustible heat source 80 is a charcoal element which is assembled proximate to the aerosol-generating substrate at the distal end 13 of the strip 11. Figure 1 Elements that are substantially identical are given the same reference numerals.
[0415] Figure 4a and 4b A second embodiment of a heated aerosol-generating article 4000a, 4000b is illustrated. The aerosol-generating substrate 4020a, 4020b comprises a first downstream rod 4021 formed from a granular plant material comprising dill seed particles and a second upstream rod 4022 formed from a granular plant material comprising primarily tobacco particles. Suitable homogenized dill seed material for use in the first downstream rod is shown in Table 1 below as one of Samples A to D. Suitable homogenized tobacco material for use in the second upstream rod is shown in Table 1 below as Sample E. Sample E comprises only tobacco particles and is included for comparative purposes only.
[0416] In each stick, the homogenized plant material is in the form of a sheet that is crimped and wrapped in filter paper (not shown). Both sheets contain additives, including glycerol as an aerosol former. Figure 4a In the embodiment shown, the rods are combined in an abutting end-to-end relationship to form a strip, and each rod has an equal length of about 6 mm. In a more preferred embodiment (not shown), the second rod is preferably longer than the first rod, for example, preferably 2 mm longer, more preferably 3 mm longer, so that the second rod is 7 or 7.5 mm long and the first rod is 5 or 4.5 mm long, to provide the desired ratio of tobacco to dill seed particles in the matrix. Figure 4b , the cellulose acetate tube support member 1030 is omitted.
[0417] Similar to Figure 1 The products 1000, 4000a, 4000b are particularly suitable for use with Figure 2 The heater shown in FIG. 2 is used in conjunction with the electrically operated aerosol generating system 2000 . Figure 1 Elements that are substantially the same as the elements in the FIG are given the same reference numerals. Figure 3 In a configuration similar to the configuration of article 1001 containing combustible heat source 1080 , a combustible heat source (not shown) may alternatively be used with the second embodiment in place of an electric heating element.
[0418] Figure 5 A third embodiment of a heated aerosol-generating article 5000 is illustrated. The aerosol-generating substrate 5020 comprises a rod formed from a first sheet of homogenised dill seed material formed from a particulate plant material including a proportion of dill seed particles and a second sheet of homogenised tobacco material comprising primarily cast leaf tobacco.
[0419] Suitable homogenized dill seed material for use as the first sheet material is shown in Table 1 below as one of Samples A to D. Suitable homogenized tobacco material for use as the second sheet material is shown in Table 1 below as Sample E. Sample E contains only tobacco particles and is included for comparative purposes only.
[0420] The second sheet is overlaid on the first sheet, and the combined sheets have been crimped, gathered, and at least partially wrapped in filter paper (not shown) to form a stick that is part of a strip. Both sheets contain additives, including glycerol as an aerosol former. Similar to Figure 1 The products 1000 and 5000 are particularly suitable for use with Figure 2 The heater shown in FIG. 2 is used in conjunction with the electrically operated aerosol generating system 2000 . Figure 1 Elements that are substantially the same as the elements in the FIG are given the same reference numerals. Figure 3In a configuration similar to the configuration of article 1001 containing combustible heat source 1080 , a combustible heat source (not shown) may alternatively be used in place of the electric heating element with the third embodiment.
[0421] Figure 6a 、 6b 6c are cross-sectional views of a filter 1050 that also includes an aerosol modifying element. Figure 6a , the filter 1050 also comprises an aerosol-modifying element in the form of spherical capsules or beads 605.
[0422] exist Figure 6a In the embodiment shown, capsules or beads 605 are embedded in filter section 601 and surrounded on all sides by filter material 603. In this embodiment, the capsule comprises an outer shell and an inner core, and the inner core contains a liquid flavoring. The liquid flavoring is used to flavor the aerosol during use of the aerosol-generating article provided with the filter. When the filter is subjected to an external force, such as when squeezed by a consumer, capsule 605 releases at least a portion of the liquid flavoring. In the embodiment shown, the capsule is generally spherical and has a substantially continuous outer shell containing the liquid flavoring.
[0423] exist Figure 6b In the embodiment of FIG, filter segment 601 includes a rod of filter material 603 and a central flavor carrying thread 607 extending through the rod of filter material 603 in a direction parallel to the longitudinal axis of filter 1050. The length of central flavor carrying thread 607 is substantially the same as the length of rod of filter material 603, such that the end of central flavor carrying thread 607 is visible at the end of filter segment 601. Figure 6b In the embodiment of the invention, the filter material 603 is cellulose acetate tow. The central flavor-bearing thread 607 is formed by a twisted pack of filter segments and is loaded with an aerosol modifier.
[0424] exist Figure 6c In the embodiment of the invention, the filter segment 601 comprises more than one rod of filter material 603, 603'. Preferably, the rods of filter material 603, 603' are formed of cellulose acetate so that they can filter the aerosol provided by the aerosol generating article. A wrapper 609 wraps around and connects the filter segments 603, 603'. Within the cavity 611 is a capsule 605 comprising an outer shell and an inner core, and the inner core contains a liquid flavoring. The capsule is otherwise similar to Figure 6a implementation plan.
[0425] Figure 77 is a cross-sectional view of an aerosol-generating substrate 1020 further comprising an elongated susceptor strip 705. The aerosol-generating substrate 1020 comprises a rod 703 formed from a sheet of homogenized dill seed material comprising tobacco particles and dill seed particles. An elongated susceptor strip 705 is embedded within the rod 703 and extends in a longitudinal direction between the upstream and downstream ends of the rod 703. During use, the elongated susceptor strip 705 heats the homogenized dill seed material by means of induction heating as described above. Example
[0426] As described above with reference to the accompanying drawings, different samples of homogenized plant material for use as an aerosol-generating substrate according to the present invention can be prepared from aqueous slurries having the compositions shown in Table 1. Sample A comprises only dill seed particles and no tobacco particles according to the present invention. Samples B to D comprise both dill seed particles and tobacco particles according to the present invention. Sample E comprises only tobacco particles and is included for comparative purposes only.
[0427] Sample A was formed using a combination of CMC binder and cellulose fibers according to the second preferred embodiment of the present invention. Sample A was prepared from an aqueous slurry containing 72.97 kg water per 100 kg slurry, with the remainder being the components in the relative amounts shown in Table 1.
[0428] Samples B through E were formed according to the first preferred embodiment of the present invention using less than 25 wt% dill seed particles and a guar gum binder. Samples B through D were prepared from an aqueous slurry containing 78-79 kg water per 100 kg slurry.
[0429] In the following tables, % DWB refers to "dry weight basis", in which case the weight percentages are calculated relative to the dry weight of the homogenized plant material. Dill seed powder can be formed from dried dill seeds, which can be ground by triple impact milling to a final D95 = 777.1 microns.
[0430] The slurry was cast onto a glass plate using a casting rod (0.6 mm), dried in an oven at 140 degrees Celsius for 7 minutes, and then dried in a second oven at 120 degrees Celsius for 30 seconds.
[0431] Table 1. Dry content of slurry
[0432]
[0433] For each of the samples A to E of homogenized plant material, a rod was produced from a single continuous sheet of homogenized plant material, each of the sheets having a width of 100 mm to 130 mm. Each sheet preferably had a thickness of about 220 microns and a mass of about 197 g / m 2The weight per square meter was approximately 131 mm. Each sheet was cut to a width of approximately 131 mm. The sheets were crimped to a height of 165 to 170 μm and rolled into rods approximately 12 mm long and 7 mm in diameter, surrounded by wrapping paper. The weight of the homogenized plant material in each rod was approximately 310 mg, and the total weight of each rod was approximately 323.6 mg.
[0434] For each rod, an aerosol-generating article having a total length of about 45 mm may be formed having a Figure 3 The structure shown in the figure includes, from the downstream end: a mouth-end cellulose acetate filter (about 7 mm long), an aerosol spacer comprising a crimped sheet of polylactic acid polymer (about 18 mm long), a hollow cellulose acetate tube (about 8 mm long) and a rod of aerosol-generating substrate.
[0435] For sample B of homogenized plant material, in which dill seed particles comprised 20% of the granulated plant material, characteristic compounds were extracted from sticks of homogenized plant material using methanol as described above. The extract was analyzed as described above to confirm the presence and measure the amount of the characteristic compounds. The results of this analysis are shown in Table 2 below, where the indicated amounts correspond to the amount per aerosol-generating article, wherein the aerosol-generating matrix of the aerosol-generating article comprised 310 mg of sample B of homogenized plant material.
[0436] For comparison purposes, the amount of the characteristic compound present in the granular plant material (dill seed granules) used to form Sample B is also shown. For the granular material, the amount indicated corresponds to the amount of the characteristic compound in a sample of granular plant material having a weight corresponding to the total weight of the granular plant material in an aerosol-generating article containing 310 mg of Sample B.
[0437] Table 2. Amounts of dill seed-specific compounds in the particulate plant material and aerosol-generating matrix
[0438]
[0439] For each of the other samples containing a certain proportion of dill seed particles, the amount of the characteristic compound can be estimated based on the values in Table 2 by assuming that the amount is proportional to the weight of the dill seed particles.
[0440] A mainstream aerosol of an aerosol-generating article incorporating an aerosol-generating matrix formed from samples A to E of homogenised plant material may be generated according to Test Method A as defined above. For each sample, the generated aerosol may be captured and analysed.
[0441] As described in detail above, according to Test Method A, commercially available The aerosol-generating article was tested using a heat-not-burn device, the Tobacco Heating System 2.2 Holder (THS2.2 Holder) (from Philip Morris Products SA). The aerosol-generating article was heated for over 30 puffs according to the Health Canada machine smoking protocol, with a puff volume of 55 ml, a puff duration of 2 seconds, and a puff interval of 30 seconds (as described in ISO / TR 19478-1:2014).
[0442] The aerosol generated during the smoking test was collected on a Cambridge filter pad and extracted with a liquid solvent. Figure 8 Suitable apparatus for generating and collecting aerosol from an aerosol-generating article is shown.
[0443] Figure 8 The aerosol generating device 111 shown is a commercially available tobacco heating device (IQOS). The contents of the mainstream aerosol generated during the Health Canada smoking test described above are collected in an aerosol collection chamber 113 on an aerosol collection line 120. The glass fiber filter mat 140 is a 44 mm Cambridge glass fiber filter mat (CFP) according to ISO 4387 and ISO 3308.
[0444] For LC-HRAM-MS analysis :
[0445] In this case, the extraction solvent 170, 170a, consisting of methanol and an internal standard (ISTD) solution, is stored in a 10 mL volume in each micro-dust detector 160, 160a. Cooling baths 161, 161a, each containing dry ice-isopropyl ether, maintain the micro-dust detectors 160, 160a at approximately -60°C. As the aerosol bubbles through the micro-dust detectors 160, 160a, the gas-vapor phase is trapped in the extraction solvent 170, 170a. In step 181, the combined solution from the two micro-dust detectors is separated into a dust detector-trapped gas-vapor phase solution 180.
[0446] In step 190, the CFP and the gas-vapor phase solution 180 captured by the dust detector are combined in a clean In step 200, total particulate matter is extracted from the CFP using a gas-vapor phase solution 180 captured by a dust analyzer (containing methanol as the solvent) by vigorous shaking (to disintegrate the CFP), vortexing for 5 minutes, and finally centrifuging (4500 g, 5 min, 10°C). An aliquot (300 μL) of the reconstituted whole aerosol extract 220 is transferred to a silanized chromatography vial and diluted with methanol (700 μL), as the extraction solvents 170 and 170a already contain an internal standard (ISTD) solution. The vial is sealed and mixed for 5 minutes using an Eppendorf ThermoMixer (5°C; 2000 rpm).
[0447] Aliquots (1.5 μL) of the diluted extract were injected and analyzed by LC-HRAM-MS in full scan mode and data-dependent fragmentation mode for compound identification.
[0448] For GCxGC-TOFMS analysis:
[0449] As described above, when preparing samples for GCxGC-TOFMS experiments, different solvents are suitable for extracting and analyzing polar, non-polar, and volatile compounds separated from whole aerosols. The experimental setup is the same as described for sample collection for LC-HRAM-MS, except as noted below.
[0450] Non-polar and polar
[0451] Extraction solvent 171, 171a, present in a volume of 10 mL, is an 80:20 v / v mixture of dichloromethane and methanol, and also contains a retention index marker (RIM) compound and a stable isotope-labeled internal standard (ISTD). Cold baths 162, 162a, each containing a dry ice-isopropanol mixture, maintain micro-dust detectors 160, 160a at approximately -78°C. As the aerosol bubbles through micro-dust detectors 160, 160a, the gas-vapor phase is trapped in extraction solvent 171, 171a. In step 182, the combined solution from the two micro-dust detectors is separated into a dust detector-trapped gas-vapor phase solution 210.
[0452] Non-polar
[0453] In step 190, the CFP and the gas-vapor phase solution 210 captured by the dust detector are combined in a clean In step 200, the total particulate matter was extracted from the CFP using a gas-vapor phase solution 210 (containing dichloromethane and methanol as solvents) captured by the dust analyzer by vigorous shaking (to disintegrate the CFP), vortexing for 5 minutes, and finally centrifuging (4500 g, 5 min, 10° C.) to separate the polar and non-polar components of the whole aerosol extract 230.
[0454] In step 250, a 10 mL aliquot 240 of the whole aerosol extract 230 is taken. In step 260, a 10 mL aliquot of water is added, and the entire sample is shaken and centrifuged. The non-polar fraction 270 is separated, dried over sodium sulfate, and analyzed by GCxGC-TOFMS in full scan mode.
[0455] polarity
[0456] ISTD and RIM compounds were added to the polar fraction 280 and then directly analyzed by GCxGC-TOFMS in full scan mode.
[0457] Each smoking replicate (n=3) contained the accumulated captured and reconstituted non-polar fraction 270 and polar fraction 280 of each sample.
[0458] Volatile components
[0459] The whole aerosol is captured using two micro-dust detectors 160 and 160a connected in series. The extraction solvent 172 and 172a, in this case, is N,N-dimethylformamide (DMF) containing a retention index marker (RIM) compound and a stable isotope-labeled internal standard (ISTD), with a volume of 10 mL in each micro-dust detector 160 and 160a. A cold bath 161 and 161a, each containing dry ice-isopropyl ether, maintains the micro-dust detectors 160 and 160a at approximately -60°C. As the aerosol is bubbled through the micro-dust detectors 160 and 160a, the gas-vapor phase is captured in the extraction solvent 170 and 170a. In step 183, the combined solution from the two micro-dust detectors is separated into a volatile-containing phase 211. The volatile-containing phase 211 is analyzed separately from the other phases and directly injected into a GCxGC-TOFMS using on-column cooled injection without further preparation.
[0460] Table 3 below shows the levels of characteristic compounds from dill seed particles in aerosols generated by aerosol-generating articles of Sample B incorporating homogenized plant material comprising 15% by weight of dill seed particles. For comparison purposes, Table 3 also shows the levels of characteristic compounds in aerosols generated by aerosol-generating articles of Sample E incorporating homogenized plant material, the homogenized tobacco material comprising only tobacco particles (and therefore not in accordance with the present invention).
[0461] Table 3. Contents of characteristic compounds in aerosol
[0462]
[0463]
[0464] Relatively high levels of the characteristic compound were measured in the aerosol generated from Sample B. The ratio of carvone to limonene was less than 10. Therefore, the level of the characteristic compound indicated the presence of dill seed particles in the sample. In contrast, for Sample E, which was tobacco-only and essentially free of dill seed particles, the level of the characteristic compound was found to be zero or close to zero.
[0465] For each of the other samples B to D containing a certain proportion of dill seed particles, the amount of the characteristic compound in the aerosol can be estimated based on the values in Table 3 by assuming that the amount is proportional to the weight of the dill seed particles in the aerosol-generating matrix from which the aerosol is generated.
[0466] Table 4 below compares the levels of certain aerosol constituents in an aerosol generated by an aerosol-generating article incorporating Sample A (20:80 ratio of dill seed to tobacco) with an aerosol generated by tobacco-only Sample E. The reduction indicated is the percentage reduction provided by replacing 20% of the tobacco particles in the homogenized material of Sample E with dill seed particles.
[0467] Table 4. Composition of aerosol
[0468]
[0469] As shown in Table 4, the aerosol generated from Sample A, which contained 20% by weight of dill seed particles based on the dry weight of the granulated plant material, resulted in a reduction in the level of formaldehyde when compared to the level of formaldehyde in the aerosol generated from Sample E, which contained 100% by weight of tobacco based on the dry weight of the granulated plant material. In addition, the aerosol generated from Sample A resulted in a reduction in the levels of several polycyclic aromatic hydrocarbons (PAHs): benzo[a]pyrene, benz[a]anthracene, and dibenzo[a,h]anthrapyrene, when compared to the aerosol generated from Sample E. In addition, the aerosol generated from Sample A resulted in a reduction in the levels of several phenolic compounds, including phenol and resorcinol.
[0470] In most cases, the reduction in the levels of these undesirable aerosol compounds provided was significantly greater than the proportional reduction expected from replacing 20% of the tobacco particles with dill seed particles. Thus, the inclusion of dill seed particles in combination with tobacco particles provided an unexpectedly high reduction in the levels of these compounds. Thus, the inclusion of dill seed particles can provide an aerosol with improved sensory attributes while reducing the levels of certain undesirable compounds in the aerosol.
Claims
1. An aerosol-generating article comprising an aerosol-generating substrate, the aerosol-generating substrate comprising a homogenized dill seed material, the homogenized dill seed material comprising dill seed particles, an aerosol-former, and a binder, wherein the aerosol-generating substrate comprises: at least 100 micrograms of carvone per gram of said substrate on a dry weight basis; and at least 2 micrograms of limonene per gram of said substrate on a dry weight basis, wherein the amount of carvone per gram of the substrate is not more than 50 times the amount of limonene per gram of the substrate.
2. An aerosol-generating article according to claim 1, wherein the aerosol-generating substrate further comprises 1 mg to 20 mg of nicotine per gram of the substrate on a dry weight basis.
3. The aerosol-generating article of claim 1 , wherein the homogenized dill seed material comprises, on a dry weight basis, 5 to 55 wt% aerosol-former and 1 to 10 wt% binder.
4. The aerosol-generating article of claim 1 , wherein the binder comprises guar gum.
5. The aerosol-generating article of claim 1, wherein the binder comprises a cellulose ether.
6. An aerosol-generating article according to claim 5, wherein the aerosol-generating substrate further comprises additional cellulose not derived from dill seed particles, wherein the additional cellulose comprises at least one of cellulose powder and cellulose fibers.
7. The aerosol-generating article of claim 1, wherein the homogenized dill seed material comprises at least 2.5 wt% dill seed particles on a dry weight basis.
8. The aerosol-generating article of claim 1, wherein the homogenized dill seed material further comprises tobacco particles and wherein the weight ratio of dill seed particles to tobacco particles is no greater than 1:
4.
9. An aerosol-generating article according to claim 1, wherein the homogenised dill seed material in the aerosol-generating substrate is in the form of cast leaves.
10. The aerosol-generating article of claim 1, wherein the homogenized dill seed material is in the form of dill seed paper.
11. An aerosol-generating article according to claim 1 , wherein upon heating the aerosol-generating substrate according to Test Method A described in ISO / TR 19478-1:2014, the generated aerosol comprises: at least 20 micrograms of carvone per gram of said substrate on a dry weight basis; and at least 2 micrograms of limonene per gram of said substrate on a dry weight basis; The amount of carvone in the aerosol per gram of the substrate is not more than 10 times the amount of limonene in the aerosol per gram of the substrate.
12. An aerosol-generating article according to claim 1 , wherein, upon heating the aerosol-generating substrate according to Test Method A described in ISO / TR 19478-1:2014, the aerosol generated by the aerosol-generating substrate comprises: Carvone in an amount of at least 0.5 micrograms per aerosol puff; and At least 0.05 micrograms of limonene per aerosol puff, wherein the aerosol has a volume of 55 ml generated by the smoking machine, and wherein the amount of carvone per aerosol is no more than 10 times the amount of limonene per aerosol.
13. An aerosol-generating substrate comprising a homogenized dill seed material comprising dill seed particles, an aerosol-forming agent, and a binder, wherein the aerosol-generating substrate comprises: at least 100 micrograms of carvone per gram of said substrate on a dry weight basis; and at least 2 micrograms of limonene per gram of said substrate on a dry weight basis, wherein the amount of carvone per gram of the substrate is not more than 50 times the amount of limonene per gram of the substrate.
14. An aerosol generating system, comprising: an aerosol generating device comprising a heating element; and An aerosol-generating article according to any one of claims 1 to 12.
15. An aerosol generated upon heating the aerosol-generating substrate according to claim 13, the aerosol comprising: Carvone in an amount of at least 0.5 micrograms per aerosol puff; and At least 0.05 micrograms of limonene per aerosol puff, wherein the aerosol produced by the smoking machine has a volume of 55 ml on one puff, and wherein the amount of carvone in the aerosol per gram of the substrate is no more than 10 times the amount of limonene in the aerosol per gram of the substrate.
16. A method of manufacturing an aerosol-generating substrate according to claim 13, the method comprising the steps of: forming a slurry comprising dill seed particles, water, an aerosol former, a binder, and optionally tobacco particles; Casting or extruding the slurry into a sheet or strip form; and The sheets or strips are dried at 80 to 160 degrees Celsius.
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