Novel aerosol-generating substrate comprising rosemary species
By using homogenized rosemary material as the aerosol generation matrix, which contains rosemary particles and specific compounds, the problem of insufficient flavor and mouthfeel in heated aerosol products is solved, resulting in an improved aerosol experience and ease of manufacturing.
Patent Information
- Application Number
- CN202180015267.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Priority Date
- 2020-02-28
- Filing Date
- 2021-02-24
- Publication Date
- 2026-08-25
- Estimated Expiration
- 2041-02-24
AI Technical Summary
Existing heated aerosol generators cannot provide a similar flavor and mouthfeel to conventional combustible cigarettes, and are difficult to manufacture easily in existing equipment.
Homogenized rosemary material is used as the aerosol generation matrix, which includes rosemary particles, aerosol forming agent and binder. Aerosol is generated by heating. Birch acid, rosmarinic acid and 12-O-methylsalicylol are preferably added to improve flavor and mouthfeel.
The generated aerosol provides improved rosemary aroma and flavor, increases mouthfeel, while reducing unwanted aerosol compounds and is easy to manufacture in existing equipment.
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Figure CN115515438B_ABST
Abstract
Description
[0001] This invention relates to an aerosol-generating matrix comprising a homogenized plant material formed from rosemary particles, and to aerosol-generating articles incorporating such an aerosol-generating matrix. The invention also relates to an aerosol derived from an aerosol-generating matrix comprising rosemary particles.
[0002] Aerosol-generating articles, which use a tobacco-containing matrix heated rather than burned, are known in the art. Typically, in such articles, aerosols are generated by transferring heat from a heat source to a physically separated aerosol-generating matrix 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 matrix via heat transfer from the heat source and entrained in the 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 a different sensory experience, such as to enhance the flavor of the aerosol. Flavoring agents can be used to deliver taste (flavor), smell (odor), or both taste and smell to a user who inhales the aerosol. Heated aerosol-generating articles containing flavoring agents are known.
[0004] It is also known to provide flavorings in conventional combustible cigarettes, which are inhaled by lighting the end of the cigarette opposite the mouthpiece, causing the tobacco stick to burn and produce inhalable smoke. One or more flavorings are typically mixed with the tobacco in the tobacco stick to provide additional flavor to the mainstream smoke as the tobacco burns. Such flavorings may be provided, for example, as essential oils.
[0005] Aerosols from regular cigarettes, containing a large number of components that interact with receptors in the mouth, provide a “full mouth” sensation, that is, a relatively full mouthfeel. As used in this article, “mouthfeel” refers to the physical sensation in the oral cavity evoked by food, beverage, or aerosol, and is distinct from taste. It is a fundamental sensory property that, along with taste and odor, determines the overall flavor of a food or aerosol.
[0006] Replicating the consumer experience offered by conventional combustible cigarettes using aerosol-generating articles in which the aerosol-generating matrix is heated rather than burned presents challenges. This is partly due to the relatively low temperatures achieved during the heating of such aerosol-generating articles, which result in a different distribution of the released volatile compounds.
[0007] It is desirable to provide a novel aerosol-generating matrix for heated aerosol-generating articles, which provides an aerosol with improved flavor and mouthfeel. It would be particularly desirable if such an aerosol-generating matrix could provide an aerosol with a sensory experience comparable to that offered by conventional combustible cigarettes.
[0008] It is also desirable to provide such an aerosol generation matrix that can be easily incorporated into aerosol generation articles and can be manufactured using existing high-speed methods and equipment.
[0009] This disclosure relates to an aerosol generating article comprising an aerosol generating matrix formed from a homogenized rosemary material containing rosemary particles. The homogenized rosemary material may contain 1% to 25% by weight of rosemary particles on a dry weight basis. The homogenized rosemary material may contain 5% to 30% by weight of an aerosol forming agent on a dry weight basis. The homogenized rosemary material may contain 1% to 10% by weight of a binder on a dry weight basis.
[0010] According to the present invention, an aerosol generating article comprising an aerosol generating matrix is provided, said aerosol generating matrix being formed from a homogenized rosemary material comprising rosemary particles. According to the present invention, the homogenized rosemary material comprises: 1% to 25% by weight of rosemary particles on a dry weight basis; 5% to 30% by weight of an aerosol forming agent on a dry weight basis; and 1% to 10% by weight of a binder on a dry weight basis.
[0011] The aerosol generating matrix preferably further comprises at least 50 micrograms of betulinic acid per gram of matrix on a dry weight basis; at least 20 micrograms of rosmarinic acid per gram of matrix on a dry weight basis; and at least 0.3 micrograms of 12-O-methylsalvinylphenol per gram of matrix on a dry weight basis.
[0012] Preferably, when the aerosol generating matrix of the aerosol generating article according to the present invention is heated according to test method A as described below, an aerosol comprising the following is generated: at least 30 micrograms of betulinic acid per gram matrix by dry weight; at least 1 microgram of rosmarinic acid per gram matrix by dry weight; and at least 1 microgram of 12-O-methylsalvinylphenol per gram matrix by dry weight.
[0013] Preferably, when the aerosol generating matrix is heated according to test method A, the aerosol generated by the aerosol generating matrix may contain at least 0.5 micrograms of betulinic acid per aspirated volume. When the aerosol generating matrix is heated according to test method A, the aerosol generated by the aerosol generating matrix may contain at least 0.01 micrograms of rosmarinic acid per aspirated volume. When the aerosol generating matrix is heated according to test method A, the aerosol generated by the aerosol generating matrix may contain at least 0.01 micrograms of 12-O-methylsalazine per aspirated volume. If generated by a smoking machine, a single aspirated volume of the aerosol is 55 ml.
[0014] This disclosure also relates to an aerosol-generating matrix formed from a homogenized rosemary material comprising rosemary particles. The homogenized plant material may contain 1% to 25% by weight of rosemary particles. The homogenized rosemary material may contain 5% to 30% by weight of an aerosol-forming agent. The homogenized rosemary material may contain 1% to 10% by weight of a binder.
[0015] According to the present invention, an aerosol generating matrix formed from homogenized rosemary material is also provided, wherein the homogenized rosemary material comprises 1% to 25% by weight of rosemary particles, 5% to 30% by weight of aerosol forming agent and 1% to 10% by weight of binder.
[0016] Preferably, the homogenized rosemary material further comprises at least 50 micrograms of betulinic acid per gram matrix, at least 20 micrograms of rosmarinic acid per gram matrix on a dry weight basis, and at least 0.3 micrograms of 12-O-methylsalazine per gram matrix on a dry weight basis.
[0017] This disclosure also relates to an aerosol generated during the heating of an aerosol-generating matrix. The aerosol may contain at least 0.5 micrograms of betulinic acid per aspiration. The aerosol may contain at least 0.01 micrograms of rosmarinic acid per aspiration. The aerosol may contain at least 0.01 micrograms of 12-O-methylsalazine per aspiration. If generated by a smoking machine, a single aspiration of the aerosol has a volume of 55 ml.
[0018] According to the present invention, an aerosol generated during heating of an aerosol-generating matrix is also provided, the aerosol comprising: at least 0.5 micrograms of betulinic acid per aspiration; at least 0.01 micrograms of rosmarinic acid per aspiration; and at least 0.01 micrograms of 12-O-methylsalmonol per aspiration, wherein, if generated by a smoking machine, a single aspiration of the aerosol has a volume of 55 ml.
[0019] The present invention also provides a method for manufacturing an aerosol-generating matrix, comprising: forming a slurry comprising rosemary particles, water, an aerosol forming agent, a binder, and optionally tobacco particles; casting or extruding the slurry into sheets or strips; and drying the sheets or strips between 80 and 160 degrees Celsius. In the case of forming an aerosol-generating matrix sheet, the sheet may optionally be cut into strips or aggregated to form strips. The sheet may optionally be pressed together prior to the aggregation step.
[0020] Unless otherwise stated, any references to the aerosol generating matrix and aerosols of the present invention below shall be considered applicable to all aspects of the present invention.
[0021] As used herein, the term "aerosol-generating article" refers to an article for generating aerosols, wherein the article comprises an aerosol-generating matrix suitable and intended to be heated or combusted to release volatile compounds that can form aerosols. A conventional cigarette is ignited when a user applies a flame to one end and inhales air through the other end. The localized heat provided by the flame and oxygen in the air inhaled through the cigarette ignites the end of the cigarette, and the resulting combustion produces inhalable smoke. In contrast, in a "heated aerosol-generating article," aerosols are generated by heating the aerosol-generating matrix rather than by burning the aerosol-generating matrix. Known heated aerosol-generating articles include, for example, electrically heated aerosol-generating articles and aerosol-generating articles in which aerosols are generated by heat transfer from a combustible fuel element or heat source to a physically separate aerosol-generating matrix.
[0022] Aerosol generating articles suitable for use in aerosol generating systems that supply aerosol forming agents to aerosol generating articles are also known. In contrast to aerosol generating matrices that carry and supply substantially all aerosol forming agents used in the formation of aerosols during operation, the aerosol generating matrix in such a system contains significantly less aerosol forming agent.
[0023] As used herein, the term "aerosol-generating matrix" refers to a matrix capable of generating volatile compounds upon heating, which can form aerosols. Aerosols generated from an aerosol-generating matrix may be visible or invisible to the human eye and may contain vapors (e.g., fine particulate matter in a gaseous state, which are typically liquid or solid at room temperature) as well as droplets of gas and condensed vapors.
[0024] As used herein, the term "homogenized plant material" encompasses any plant material formed by the agglomeration of plant particles. For example, sheets or webs of homogenized plant material used in the aerosol-generating matrix of the present invention can be formed by agglomerating plant material particles obtained by crushing, grinding, or grinding rosemary plant material and optionally tobacco material such as tobacco leaves and stems. Homogenized plant material can be produced by casting, extrusion, papermaking processes, or any other suitable process known in the art.
[0025] As used herein, the term "homogenized rosemary material" refers to a homogenized plant material that optionally contains rosemary particles in combination with tobacco particles. The term "homogenized tobacco material" refers to a homogenized plant material that contains tobacco particles but not rosemary particles, and is therefore not according to the invention.
[0026] As used in this article, the term "rosemary granules" encompasses the term originating from... Rosemary (Rosmarinus officinalis) Particles, preferably derived from Rosemary (Lamiaceae family) The dried leaves and flower granules of plants. rosemary It is a woody, perennial herb with fragrant, evergreen, needle-like leaves and white, pink, purple, or blue flowers. Native to the Mediterranean region and Asia, this plant is also known as sage or rosemary. Salvia rosmarinus) .
[0027] Rosemary is commonly used as a flavoring. Its fresh or dried leaves, with their characteristic aroma, form the basis of traditional Mediterranean cuisine and complement many cooked dishes. Rosemary extract is frequently used in perfumes, shampoos, cleaning products, and air fresheners.
[0028] In contrast, rosemary essential oil is a distillate, and rosmarinic acid is a compound derived from rosemary. These are not considered rosemary granules, nor are they included in the percentage of granular plant material.
[0029] This invention provides an aerosol-generating article incorporating an aerosol-generating matrix formed from a homogenized plant material containing rosemary particles—referred to herein as "homogenized rosemary material." The invention also provides an aerosol derived from such an aerosol-generating matrix. The inventors have discovered that by introducing rosemary particles into an aerosol-generating matrix, it is advantageous to produce aerosols that provide a novel sensory experience. Such aerosols offer a unique flavor and can provide an increased level of mouthfeel.
[0030] Furthermore, the inventors have discovered that it is advantageous to produce aerosols with improved rosemary aroma and flavor compared to aerosols produced by adding rosemary additives such as rosemary oil. Rosemary oil (Chemical Abstracts Service registration number 8000-25-7) is obtained by steam distillation of the young shoots and tips of the rosemary plant and has a flavoring composition different from that of rosemary granules, presumably because the distillation process may selectively remove or retain certain flavorings. 1,8-Cineole, α-pinene, and camphor are the main components of rosemary oil obtained from rosemary plants grown in Spain and North Africa. Trace amounts of verbenane have also been found in North African rosemary oil, but in slightly higher amounts in Spanish rosemary oil.
[0031] Furthermore, in some of the aerosol-generating matrices provided in this article, sufficient levels of rosemary particles can be introduced to provide the desired rosemary flavor while maintaining sufficient tobacco material to provide consumers with the desired nicotine levels.
[0032] Furthermore, it has been surprisingly found that including rosemary particles in the aerosol-generating matrix provides a significant reduction in certain undesirable aerosol compounds compared to aerosols generated from an aerosol-generating matrix containing 100% tobacco particles but no rosemary particles.
[0033] The presence of rosemary in homogenized plant materials (such as dwarf rosemary) can be definitively identified by DNA barcoding. The method of DNA barcoding based on the nuclear gene ITS2, rbcL, and matK system, and the plastid gene spacer trnH-psbA, is 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. PLoSONE 5(1): e8613; Hollingsworth PM, Graham SW, Little DP (2011) Choosing and Using a Plant DNA Barcode. PLoS ONE 6(5): e19254).
[0034] The inventors have reanalyzed and characterized aerosols generated by the aerosol-generating matrix of the present invention, which incorporates rosemary particles and mixtures of rosemary and tobacco particles, and compared these aerosols with those generated by existing aerosol-generating matrices formed from tobacco materials without rosemary particles. Based on this, the inventors have been able to identify a group of “characteristic compounds” that are present in the aerosols and derived from rosemary particles. Therefore, the detection of these characteristic compounds within a specific weight range of the aerosol can be used to identify aerosols derived from aerosol-generating matrices containing rosemary particles. These characteristic compounds are clearly not present in aerosols generated from tobacco materials. Furthermore, the proportion of characteristic compounds within the aerosol and the ratios between characteristic compounds clearly indicate the use of rosemary plant material rather than rosemary oil. Similarly, the presence of these characteristic compounds in a specific proportion within the aerosol-generating matrix indicates the inclusion of rosemary particles in the matrix.
[0035] Specifically, the defined levels of characteristic compounds within the matrix and aerosol are specific to the rosemary particles present within the homogenized rosemary material. The level of each characteristic compound depends on the manner in which the rosemary particles are processed during the production of the homogenized rosemary material. These levels also depend on the composition of the homogenized rosemary material and, in particular, will be influenced by the levels of other components within the homogenized rosemary material. The levels of characteristic compounds within the homogenized rosemary material will differ from the levels of the same compounds in the starting rosemary material. They will also differ from the levels of characteristic compounds in materials containing rosemary particles but not as defined herein according to the invention.
[0036] To characterize aerosols, the inventors utilized complementary non-targeted differential screening (NTDS), which employs liquid chromatography coupled to high-resolution precision mass spectrometry (LC-HRAM-MS) in parallel with two-dimensional gas chromatography (GCxGC-TOFMS) coupled to time-of-flight mass spectrometry.
[0037] Non-targeted screening (NTS) is a key method for characterizing the chemical composition of complex matrices. It involves matching the features of unknown detected compounds with a spectral database (suspicion screening analysis [SSA]), or, if no prior knowledge is available for matching, using information obtained through, for example, first-order fragmentation (MS / MS), and comparing it with information from a compound database. computer Predictive fragment matching (non-targeted analysis [NTA]) is used to elucidate the structure of unknowns. It enables the simultaneous measurement and semi-quantification of a large number of small molecules from a sample using unbiased methods.
[0038] If, as described above, the focus is on comparing two or more aerosol samples to evaluate any significant differences in chemical composition between the samples in an unsupervised manner, or if group-related predispositions between sample groups are available, then non-targeted differential screening (NTDS) can be performed. A complementary differential screening method has been applied using liquid chromatography coupled to high-resolution precision mass spectrometry (LC-HRAM-MS) in parallel with two-dimensional gas chromatography (GCxGC-TOFMS) coupled to time-of-flight mass spectrometry to ensure comprehensive analytical coverage for identifying the most relevant differences in aerosol composition between aerosols derived from products containing 100 wt% rosemary as particulate plant material and those derived from products containing 100 wt% tobacco as particulate plant material.
[0039] Aerosols are generated and collected using the equipment and methods described in detail below.
[0040] Using Thermo QExactive TM High-resolution mass spectrometry was used for LC-HRAM-MS analysis in full scan and data-dependent modes. A total of three different methods were employed to cover a wide range of substances with different ionization properties and compound classes. RP chromatography was used to analyze samples using heated electrospray ionization (HESI) in both positive and negative modes, and atmospheric pressure chemical ionization (APCI) in positive mode. These methods are described by Arndt, D. et al. , "Indepth characterization of chemical differences between heat-not-burn tobaccoproducts and cigarettes using LC-HRAM-MS-based non-targeted differentialscreening" (DOI:10.13140 / RG.2.2.11752.16643); Wachsmuth, C. et al. , “Comprehensive chemical characterization of complex matrices through integration of multiple analytical modes and databases for LC-HRAM-MS-basednon-targeted screening” (DOI: 10.13140 / RG.2.2.12701.61927); and “Buchholz, C. wait peopleThe results, “Increasing confidence for compound identification by fragmentation database and in silico fragmentation comparison with LC-HRAM-MS-based non-targeted screening of complex matrices” (DOI: 10.13140 / RG.2.2.17944.49927), are from the 66th ASMS Conference on Mass Spectrometry and Allied Topics (San Diego, USA (2018)). These methods are also described by Arndt, D. et al. , “Acomplex matrix characterization approach, applied to cigarette smoke, that integrates multiple analytical methods and compound identification strategies for non-targeted liquid chromatography with high-resolution massspectrometry” (DOI: 10.1002 / rcm.8571).
[0041] GCxGC-TOFMS analysis was performed using an Agilent GC 6890A or 7890A instrument equipped with an automated liquid sampler (model 7683B) and a thermal regulator coupled to a LECO Pegasus 4D™ mass spectrometer, employing three different methods for nonpolar, polar, and highly volatile compounds within aerosols. 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.
[0042] The results of the analytical methods provide information about the main compounds causing the differences in aerosols generated by these articles. The focus of non-targeted differential screening using the analytical platforms LC-HRAM-MS and GCxGC-TOFMS is on compounds present in greater quantities in the aerosols of samples containing 100% rosemary particles according to the present invention, relative to comparative samples containing 100% tobacco particles as the aerosol-generating matrix. The NTDS method is described in the aforementioned literature.
[0043] Based on this information, the inventors were able to identify specific compounds within the aerosol that could be considered "characteristic compounds" originating from rosemary particles in the matrix. Characteristic compounds unique to rosemary include, but are not limited to: betulinic acid ((3β)-3-hydroxy-lupin-20(29)-ene-28-acid, chemical formula: C 30 H 48 O3, Chemical Abstracts Service registration number 472-15-1); Rosmarin (4,5-dihydroxy-12,12-dimethyl-6-(propane-2-yl)tricyclic [9.4.0.0³, 8 [15-C-3,5,7-trien-2-one], chemical formula: C 20 H 28 O3, Chemical Abstracts Service registration number 1729-95-2; and 12-O-methylcaryophyllin, chemical formula: C 21 H 28 O4, Chemical Abstracts Service registration number 85514-27-8.
[0044] For the purposes of this invention, a sample of an aerosol-generating matrix can be targeted for screening to identify the presence and amount of each characteristic compound in the matrix. This targeted screening method is described below. As described, characteristic compounds can be detected and measured in the aerosol-generating matrix and in aerosols derived from the aerosol-generating matrix.
[0045] As defined above, the aerosol-generating article of the present invention comprises an aerosol-generating matrix formed from a homogenized rosemary material containing rosemary particles. Because it contains rosemary particles, the aerosol-generating matrix contains a certain proportion of the "characteristic compounds" of rosemary, as described above. In particular, the aerosol-generating matrix preferably contains at least 50 micrograms of betulinic acid per gram matrix, at least 20 micrograms of rosmarinic acid per gram matrix, and at least 0.3 micrograms of 12-O-methylsalaflavin per gram matrix, based on dry weight.
[0046] By defining the aerosol-generating matrix relative to the desired levels of characteristic compounds, consistency between products can be ensured despite potential variations in the levels of characteristic compounds in the raw materials. This advantageously enables more effective control over product quality.
[0047] Preferably, the aerosol-generating matrix comprises at least about 100 micrograms of betulinic acid per gram of matrix, more preferably at least about 250 micrograms of betulinic acid per gram of matrix, and even more preferably at least about 500 micrograms of betulinic acid per gram of matrix, based on dry weight. Alternatively or additionally, the aerosol-generating matrix preferably comprises no more than about 2000 micrograms of betulinic acid per gram of matrix, more preferably no more than about 1750 micrograms of betulinic acid per gram of matrix, even more preferably no more than about 1500 micrograms of betulinic acid per gram of matrix, and even more preferably no more than about 1000 micrograms of betulinic acid per gram of matrix, based on dry weight.
[0048] For example, the aerosol generating matrix may contain betulinic acid per gram of matrix at a dry weight of about 50 micrograms to about 2000 micrograms, or about 100 micrograms to about 1750 micrograms, or about 250 micrograms to about 1500 micrograms, or about 500 micrograms to about 100 micrograms.
[0049] Preferably, the aerosol-generating matrix comprises at least about 50 micrograms of rosmarinic acid per gram of matrix, more preferably at least about 100 micrograms of rosmarinic acid per gram of matrix, and even more preferably at least about 200 micrograms of rosmarinic acid per gram of matrix, based on dry weight. Alternatively or additionally, the aerosol-generating matrix preferably comprises no more than about 1000 micrograms of rosmarinic acid per gram of matrix, more preferably no more than about 800 micrograms of rosmarinic acid per gram of matrix, more preferably no more than about 700 micrograms of rosmarinic acid per gram of matrix, and even more preferably no more than about 600 micrograms of rosmarinic acid per gram of matrix, based on dry weight.
[0050] For example, the aerosol generating matrix may contain about 20 micrograms to about 1,000 micrograms of rosmarinic acid per gram of matrix, or about 50 micrograms to about 800 micrograms of rosmarinic acid per gram of matrix, or about 100 micrograms to about 700 micrograms of rosmarinic acid per gram of matrix, or about 200 micrograms to about 600 micrograms of rosmarinic acid per gram of matrix, on a dry weight basis.
[0051] Preferably, the aerosol-generating matrix comprises at least about 1 microgram of 12-O-methylcaryophyllene per gram of matrix, more preferably at least about 2 micrograms of 12-O-methylcaryophyllene per gram of matrix, and even more preferably at least about 4 micrograms of 12-O-methylcaryophyllene per gram of matrix, based on dry weight. Alternatively or additionally, the aerosol-generating matrix preferably comprises no more than about 20 micrograms of 12-O-methylcaryophyllene per gram of matrix, more preferably no more than about 18 micrograms of 12-O-methylcaryophyllene per gram of matrix, even more preferably no more than about 15 micrograms of 12-O-methylcaryophyllene per gram of matrix, and even more preferably no more than about 12 micrograms of 12-O-methylcaryophyllene per gram of matrix, based on dry weight.
[0052] For example, the aerosol generating matrix may contain between about 0.3 micrograms and about 20 micrograms of 12-O-methylcaryophyllin per gram of matrix on a dry weight basis, or between about 1 microgram and about 18 micrograms of 12-O-methylcaryophyllin per gram of matrix, or between about 2 micrograms and about 15 micrograms of 12-O-methylcaryophyllin per gram of matrix, or between about 4 micrograms and about 12 micrograms of 12-O-methylcaryophyllin per gram of matrix.
[0053] Preferably, the ratio of characteristic compounds in the aerosol-generating matrix is such that the amount of betulinic acid / g matrix is at least 2 times the amount of rosmarinic acid / g matrix, more preferably at least 2.5 times the amount of rosmarinic acid / g matrix, and even more preferably at least 3 times the amount of rosmarinic acid / g matrix.
[0054] This ratio of betulinic acid to rosmarinic acid is unique to the introduction of rosemary particles into the aerosol-generating matrix.
[0055] Preferably, the aerosol generating matrix contains more than 0.5% by weight of 1,8-cineole on a dry weight basis. More preferably, the aerosol generating matrix contains more than about 1% by weight of 1,8-cineole on a dry weight basis.
[0056] As defined above, the present invention also provides an aerosol generating article comprising an aerosol generating matrix formed from a homogenized rosemary material containing rosemary particles, wherein an aerosol containing a "characteristic compound" of rosemary is generated when the aerosol generating matrix is heated.
[0057] For the purposes of this invention, an aerosol-generating matrix is heated according to "Test Method A". In Test Method A, under the Health Canada machine smoking protocol, an aerosol-generating article incorporating the aerosol-generating matrix is heated in a tobacco heating system 2.2 retainer (THS2.2 retainer). For the purposes of performing Test Method A, an aerosol-generating matrix is provided in an aerosol-generating article compatible with the THS2.2 retainer.
[0058] The tobacco heating system 2.2 retainer (THS2.2 retainer) corresponds to a 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 used in conjunction with the IQOS device are also commercially available.
[0059] The Health Canada smoking protocol is a well-defined and accepted smoking protocol as defined in HealthCanada 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 aerosols are collected from the sample aerosol-generating matrix, with a draw volume of 55 mm, a draw duration of 2 seconds, and a draw interval of 30 seconds. If ventilation is present, all ventilations are blocked.
[0060] Therefore, in the context of this invention, the phrase "when heating the aerosol-generating matrix according to test method A" means heating the aerosol-generating matrix in a THS 2.2 holder under the Health Canada machine smoking protocol as defined in Health Canada 2000 - Tobacco Product Information Regulation SOR / 2000-273, Plan 2, published by the Ministry of Justice Canada, which is described in ISO / TR 19478-1:2014.
[0061] For the purposes of the analysis, aerosols generated by the heated aerosol-generating matrix are captured using suitable equipment, depending on the analytical method to be used. In a suitable method for producing samples for LC-HRAM-MS analysis, the particulate phase is captured using a conditioned 44 mm Cambridge glass fiber filter pad (according to ISO 3308) and a filter retainer (according to ISO 4387 and ISO 3308). The remaining gas phase is collected downstream of the filter pad using two consecutive micro-dust collectors (20 mL each), each containing methanol and an internal standard (ISTD) solution (10 mL), maintained at -60°C using a dry ice-isopropanol mixture. The captured particulate and gas phases are then recombined and extracted using methanol from the micro-dust collectors by shaking the sample, vortexing for 5 min, and centrifuging (4500 g, 5 min, 10°C). The resulting extract is diluted with methanol and mixed in an Eppendorf ThermoMixer (5°C, 2000 rpm). Characteristic compounds were identified by analyzing test samples from extracts using LC-HRAM-MS in a combined full-scan and data-dependent fracture mode. For the purposes of this invention, LC-HRAM-MS analysis is suitable for the identification and quantification of betulinic acid, rosmarinic acid, and 12-O-methylcaryophyllene.
[0062] 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, nonpolar, and volatile compounds separated from the whole aerosol.
[0063] For both nonpolar and polar compounds, a conditioned 44 mm Cambridge glass fiber filter pad (according to ISO 3308) and filter retainer (according to ISO 4387 and ISO 3308) were used, and the entire aerosol was collected using two micro-dust analyzers connected in series and sealed. Each micro-dust analyzer (20 mL) contained 10 mL of dichloromethane / methanol (80:20 v / v) containing an internal standard (ISTD) and a retention index label (RIM) compound. The micro-dust analyzers were maintained at -80 °C using a dry ice-isopropanol mixture. To analyze nonpolar compounds, the particulate phase of the entire aerosol was extracted from the glass fiber filter pad using the contents of the micro-dust analyzer. Water was added to an aliquot (10 mL) of the resulting extract, and the sample was shaken and centrifuged as described above. The dichloromethane layer was separated, dried with sodium sulfate, and analyzed by GCxGC-TOFMS in full scan mode. To analyze polar compounds, the remaining aqueous layer prepared from the nonpolar sample described above was used. ISTD and RIM compounds were added to the aqueous layer and then directly analyzed in full scan mode by GCxGC-TOFMS.
[0064] For volatile compounds, total aerosols were collected using two tandemly connected and sealed microparticle dust collectors (20 mL), each filled with 10 mL of N,N-dimethylformamide (DMF) containing ISTD and RIM compounds. The microparticle dust collectors were maintained at -50°C to -60°C using a dry ice-isopropanol mixture. After collection, the contents of the two microparticle dust collectors were combined and analyzed by GCxGC-TOFMS in full scan mode.
[0065] For the purposes of this invention, GCxGC-TOFMS analysis is suitable for the identification and quantification of 12-O-methylsarstilbenol.
[0066] When the aerosol generating matrix of the present invention is heated according to test method A, the aerosol generated is preferably characterized by the amount and ratio of the characteristic compounds betulinic acid, rosmarinic acid and 12-O-methylsalpinx as defined above.
[0067] Preferably, in the aerosol generating article comprising the aerosol generating matrix as described above, when the aerosol generating matrix is heated according to test method A, an aerosol comprising the following is generated: at least 30 micrograms of betulinic acid per gram of matrix on a dry weight basis; at least 1 microgram of rosmarinic acid per gram of matrix on a dry weight basis; and at least 1 microgram of 12-O-methylsalvinyl alcohol per gram of matrix on a dry weight basis.
[0068] The range defines the amount of each characteristic compound in the aerosol generated per gram of aerosol-generating matrix (also referred to herein as the "matrix"). This is equal to the total amount of characteristic compounds measured in the aerosol collected during Test Method A divided by the dry weight of the aerosol-generating matrix before heating.
[0069] When heating the aerosol-generating matrix according to test method A, it is preferable to generate an aerosol containing at least about 30 micrograms of betulinic acid per gram of matrix on a dry weight basis.
[0070] More preferably, the aerosol generated from the aerosol generating matrix according to the invention comprises at least about 100 micrograms of betulinic acid per gram of matrix, on a dry weight basis. Even more preferably, the aerosol generated from the aerosol generating matrix according to the invention comprises at least about 250 micrograms of betulinic acid per gram of matrix, on a dry weight basis. Alternatively or additionally, the aerosol generated from the aerosol generating matrix preferably comprises up to about 1500 micrograms of betulinic acid per gram of matrix, on a dry weight basis. More preferably, the aerosol generated from the aerosol generating matrix comprises up to about 1000 micrograms of betulinic acid per gram of matrix, on a dry weight basis. Even more preferably, the aerosol generated from the aerosol generating matrix comprises up to about 800 micrograms of betulinic acid per gram of matrix, on a dry weight basis.
[0071] When heating the aerosol-generating matrix according to test method A, an aerosol is generated that preferably contains at least about 1 microgram of rosmarinic acid per gram of matrix on a dry weight basis.
[0072] Preferably, the aerosol generated from the aerosol generating matrix according to the invention further comprises at least about 10 micrograms of rosmarinic acid per gram of matrix, based on dry weight. More preferably, the aerosol generated from the aerosol generating matrix according to the invention comprises at least about 25 micrograms of rosmarinic acid per gram of matrix, based on dry weight. Alternatively or additionally, the aerosol generated from the aerosol generating matrix preferably comprises up to about 100 micrograms of rosmarinic acid per gram of matrix, based on dry weight. More preferably, the aerosol generated from the aerosol generating matrix comprises up to about 75 micrograms of rosmarinic acid per gram of matrix, based on dry weight. Even more preferably, the aerosol generated from the aerosol generating matrix comprises up to about 50 micrograms of rosmarinic acid per gram of matrix, based on dry weight.
[0073] When heating the aerosol-generating matrix according to test method A, an aerosol is generated that preferably contains at least about 1 microgram of 12-O-methylsarstilin per gram of matrix on a dry weight basis.
[0074] Preferably, the aerosol generated from the aerosol generating matrix according to the invention comprises at least about 10 micrograms of 12-O-methylsarcophenolate per gram of matrix, based on dry weight. Even more preferably, the aerosol generated from the aerosol generating matrix according to the invention comprises at least about 25 micrograms of 12-O-methylsarcophenolate per gram of matrix, based on dry weight. Alternatively or additionally, the aerosol generated from the aerosol generating matrix preferably comprises up to about 100 micrograms of 12-O-methylsarcophenolate per gram of matrix, based on dry weight. More preferably, the aerosol generated from the aerosol generating matrix comprises up to about 75 micrograms of 12-O-methylsarcophenolate per gram of matrix, based on dry weight. Even more preferably, the aerosol generated from the aerosol generating matrix comprises up to about 50 micrograms of 12-O-methylsarcophenolate per gram of matrix, based on dry weight.
[0075] In some embodiments, the aerosol generated from the aerosol generating matrix according to the invention comprises at least 30 micrograms of betulinic acid per gram of matrix on a dry weight basis; at least 1 microgram of rosmarinic acid per gram of matrix on a dry weight basis; and at least 1 microgram of 12-O-methylsalazine per gram of matrix on a dry weight basis.
[0076] Preferably, the aerosol generated from the aerosol generating matrix according to the invention during test method A further comprises at least about 0.1 micrograms of nicotine per gram of matrix, more preferably at least about 1 microgram of nicotine per gram of matrix, and even more preferably at least about 2 micrograms of nicotine per gram of matrix. Preferably, the aerosol comprises at most about 10 micrograms of nicotine per gram of matrix, more preferably at most about 7.5 micrograms of nicotine per gram of matrix, and even more preferably at most about 4 micrograms of nicotine per gram of matrix. For example, the aerosol may comprise about 0.1 micrograms to about 10 micrograms of nicotine per gram of matrix, or about 1 microgram to about 7.5 micrograms of nicotine per gram of matrix, or about 2 micrograms to about 4 micrograms of nicotine per gram of matrix. In some embodiments of the invention, the aerosol may contain zero micrograms of nicotine.
[0077] Various methods known in the art can be used to measure the amount of nicotine in aerosols.
[0078] Carbon monoxide may also be present in the aerosol generated by the aerosol generating matrix according to the invention during test method A, and can be measured and used for further characterization of the aerosol. Nitrogen oxides, such as nitric oxide and nitrogen dioxide, may also be present in the aerosol, and can be measured and used for further characterization of the aerosol.
[0079] According to the present invention, the aerosol generated from the aerosol generating matrix during test method A preferably has at least 5 times the amount of betulinic acid per gram of matrix, preferably rosmarinic acid per gram of matrix.
[0080] More preferably, during test method A, the amount of betulinic acid in the aerosol generated from the aerosol generating matrix is at least 10 times the amount of rosmarinic acid per gram of matrix, such that the ratio of betulinic acid to rosmarinic acid is at least 10:1. Even more preferably, during test method A, the amount of betulinic acid in the aerosol generated from the aerosol generating matrix is at least 20 times the amount of rosmarinic acid per gram of matrix, such that the ratio of betulinic acid to rosmarinic acid is at least 20:1.
[0081] In a preferred embodiment, the amount of betulinic acid in the aerosol generated from the aerosol generating matrix during test method A is such that the ratio of betulinic acid to rosmarinic acid is 5:1 to 20:1.
[0082] The defined ratio of betulinic acid to rosmarinic acid characterizes aerosols derived from rosemary particles. In contrast, the ratio of betulinic acid to rosmarinic acid would be significantly different in aerosols produced from rosemary oil.
[0083] The aerosol generated from the aerosol generating matrix according to the invention during test method A may also contain at least about 5 mg of aerosol forming agent per gram of aerosol generating matrix, or at least about 10 mg of aerosol per gram of matrix, or at least about 15 mg of aerosol forming agent per gram of matrix. Alternatively or additionally, the aerosol may contain up to about 30 mg of aerosol forming agent per gram of matrix, or up to about 25 mg of aerosol forming agent per gram of matrix, or up to about 20 mg of aerosol forming agent per gram of matrix. For example, the aerosol may contain about 5 mg to about 30 mg of aerosol forming agent per gram of matrix, or about 10 mg to about 25 mg of aerosol forming agent per gram of matrix, or about 15 mg to about 20 mg of aerosol forming agent per gram of matrix. In an alternative embodiment, the aerosol may contain less than 5 mg of aerosol forming agent per gram of matrix. For example, this may be suitable if the aerosol forming agent is provided separately within the aerosol generating article or aerosol generating apparatus.
[0084] Suitable aerosol forming agents for use in this invention are described below.
[0085] Various methods known in the art can be used to measure the amount of aerosol forming agent in aerosols.
[0086] As described above, the presence of characteristic compounds in the aerosol in defined amounts and ratios indicates the presence of rosemary particles in the homogenized rosemary material forming the aerosol-generating matrix.
[0087] Preferably, the rosemary granules contain at least about 0.5 ml of volatile oil per 100 g, more preferably at least about 0.55 ml of volatile oil per 100 g. The essential oil content of the rosemary granules can be determined using steam distillation, as described in ISO 6571:2008. This provides an indication of the essential oil content of the rosemary granules.
[0088] Preferably, the aerosol generating matrix according to the present invention comprises homogenized rosemary material, said homogenized rosemary material comprising at least about 2.5% by weight of rosemary particles on a dry weight basis. Preferably, the granular plant material comprises at least about 3% by weight of rosemary particles on a dry weight basis, more preferably at least about 4% by weight of rosemary particles, more preferably at least about 5% by weight of rosemary particles, more preferably at least about 6% by weight of rosemary particles, more preferably at least about 7% by weight of rosemary particles, more preferably at least about 8% by weight of rosemary particles, more preferably at least about 9% by weight of rosemary particles, and more preferably at least about 10% by weight of rosemary particles.
[0089] In some embodiments of the invention, the plant particles forming the homogenized rosemary material may comprise at least 98% by weight, at least 95% by weight, or at least 90% by weight of rosemary particles based on the dry weight of the plant particles. In such embodiments, the aerosol-generating matrix thus comprises rosemary particles, while substantially no other plant particles. For example, the plant particles forming the homogenized rosemary material may comprise about 100% by weight of rosemary particles.
[0090] In an alternative embodiment of the invention, as described below, the homogenized rosemary material may comprise a combination of rosemary particles and tobacco particles.
[0091] In the following description of the invention, the term "granular plant material" is used collectively to refer to plant material particles used to form homogenized plant material. Granular plant material may consist essentially of rosemary particles, or may be a mixture of rosemary particles and tobacco particles.
[0092] The homogenized rosemary material may contain up to about 25% by weight of rosemary particles on a dry weight basis. Preferably, the homogenized rosemary material contains up to about 24% by weight of rosemary particles on a dry weight basis, more preferably up to about 80% by weight of rosemary particles, more preferably up to about 23% by weight of rosemary particles, more preferably up to about 22% by weight of rosemary particles, and more preferably up to about 20% by weight of rosemary particles.
[0093] For example, the homogenized rosemary material may contain about 2.5% to about 24% of rosemary particles on a dry weight basis, or about 4% to about 24% of rosemary particles, or about 5% to about 23% of rosemary particles, or about 6% to about 22% of rosemary particles, or about 8% to about 21% of rosemary particles, or about 10% to about 20% of rosemary particles.
[0094] As stated above, the inventors have identified numerous “characteristic compounds” that are unique to the rosemary plant and thus indicate the presence of rosemary plant particles within the aerosol-generating matrix.
[0095] The amount of characteristic compounds expected to be present in pure rosemary granules differs from that present in the aerosol-forming matrix. The matrix preparation process, involving hydration in a slurry or suspension and drying at elevated temperatures, as well as the presence of other components such as aerosol-forming agents, will differentially alter the amount of each characteristic compound. The integrity of the rosemary granules and the stability of the compounds during manufacturing, under temperature and manipulation, will also affect the final amount of compounds present in the matrix. Therefore, it is envisioned that the ratio of characteristic compounds to each other will differ after rosemary granules are introduced into the matrix in various physical forms, such as sheets, strips, and particles.
[0096] The presence of rosemary within the aerosol-generating matrix and the proportion of rosemary provided within the matrix can be determined by measuring the amount of characteristic compounds within the matrix and comparing it with the corresponding amount of characteristic compounds in pure rosemary material. The presence and amount of characteristic compounds can be determined using any suitable technique known to those skilled in the art.
[0097] In a suitable technique, 250 mg of the aerosol-generating matrix sample was mixed with 5 mL of methanol and extracted by shaking, vortexing for 5 min, and centrifugation (4500 g, 5 min, 10 °C). Aliquots (300 μL) of the extract were transferred to silanized chromatographic vials and diluted with methanol (600 μL) and internal standard (ISTD) solution (100 μL). The vials were sealed and mixed for 5 min using an Eppendorf ThermoMixer (5 °C; 2000 rpm). The test sample from the resulting extract was analyzed by LC-HRAM-MS in a combined full scan mode and data-dependent fracture mode to identify characteristic compounds.
[0098] In some implementations, the homogenized rosemary material also includes up to about 75% by weight of tobacco particles on a dry weight basis.
[0099] For example, the homogenized rosemary material preferably contains about 40% to about 75% tobacco particles on a dry weight basis, more preferably about 45% to about 70% tobacco particles, and even more preferably about 50% to about 65% tobacco particles.
[0100] In some embodiments, the homogenized rosemary material comprises about 5% to about 20% by weight of rosemary particles and about 55% to about 70% by weight of tobacco particles on a dry weight basis.
[0101] The weight ratio of rosemary particles to tobacco particles in the granular plant material forming the homogenized rosemary material can vary depending on the desired flavor profile and aerosol composition. In a particularly preferred embodiment, the homogenized rosemary material comprises a weight ratio of rosemary particles to tobacco particles of no more than about 1:4. This means that the rosemary particles account for no more than 20% of the total granular plant material. More preferably, the homogenized rosemary material comprises a weight ratio of rosemary particles to tobacco particles of no more than 1:5, and more preferably no more than 1:6.
[0102] For example, in a first preferred embodiment, the weight ratio of rosemary particles to tobacco particles is 1:4. This 1:4 ratio corresponds to granular plant material consisting of approximately 20% by weight of rosemary particles and approximately 80% by weight of tobacco particles. For homogenized rosemary material formed from approximately 75% by weight of granular plant material, this is equivalent to approximately 15% by weight of rosemary particles and approximately 60% by weight of tobacco particles in the homogenized rosemary material on a dry weight basis.
[0103] In another embodiment, the homogenized rosemary material comprises rosemary particles and tobacco particles in a weight ratio of 1:9. In yet another embodiment, the homogenized rosemary material comprises rosemary particles and tobacco particles in a weight ratio of 1:30.
[0104] Referring to this invention, the term "tobacco pellet" describes tobacco Particles of any plant member of the genus *Tobacco*. The term "tobacco particles" includes ground or pulverized tobacco leaves, ground or pulverized tobacco stems, tobacco dust, tobacco debris, and other particulate tobacco byproducts formed during the processing, handling, and transportation of tobacco. In a preferred embodiment, tobacco particles are substantially entirely derived from tobacco leaves. In contrast, isolated nicotine and nicotine salts are compounds derived from tobacco but are not considered tobacco particles for the purposes of this invention and are not included in the percentage of particulate plant material.
[0105] Tobacco pellets can be prepared from one or more tobacco plants. Any type of tobacco can be used in the blend. Examples of tobacco types that can be used include, but are not limited to, sun-cured tobacco, flue-cured tobacco, burley tobacco, Maryland tobacco, Oriental tobacco, Virginia tobacco, and other specialty tobaccos.
[0106] Flue-curing is a method of drying tobacco, particularly Virginia tobacco. During the curing process, heated air circulates through densely packed tobacco leaves. In the first stage, the leaves turn yellow and wilt. In the second stage, the leaf blades are completely dried. In the third stage, the stems are completely dried.
[0107] Burley tobacco plays an important role in many tobacco blends. It has a distinctive flavor and aroma and is also capable of absorbing large amounts of casing.
[0108] Oriental tobacco is a type of tobacco characterized by small leaves and high aromatic quality. However, its flavor is milder than that of other tobaccos, such as Burley tobacco. Therefore, a relatively small proportion of Oriental tobacco is typically used in tobacco blends.
[0109] Kasturi, Madura, and Jatim are all usable subtypes of sun-cured tobacco. Preferably, Kasturi tobacco and flue-cured tobacco can be used in a mixture to produce tobacco pellets. Therefore, the tobacco pellets in the granular plant material can include a mixture of Kasturi tobacco and smoked 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 on a dry weight basis, 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. When the aerosol-generating matrix contains a combination of tobacco particles and rosemary particles, it is preferable to use tobacco with a higher nicotine content to maintain a nicotine level similar to that of a typical aerosol-generating matrix without rosemary particles, because otherwise the total amount of nicotine would be reduced due to the replacement of tobacco particles with rosemary particles.
[0111] Because it contains tobacco particles, the aerosol-generating matrix of such embodiments and the aerosol generated from the aerosol-generating matrix of such embodiments contain a certain proportion of the "characteristic compounds" of tobacco. Characteristic compounds generated from tobacco include, but are not limited to, neonicotinoids, cotinine, and damascenone. Specifically, the aerosol-generating matrix preferably contains at least about 60 micrograms of cotinine per gram of matrix and at least about 10 micrograms of damascenone per gram of matrix. Alternatively or additionally, the aerosol-generating matrix preferably contains at most about 150 micrograms of cotinine per gram of matrix and at most about 25 micrograms of damascenone per gram of matrix.
[0112] When the aerosol generating matrix is heated according to Test Method A, the aerosol generated from the aerosol generating matrix preferably contains at least about 15 micrograms of neonicotinoid / matrix, at least about 8 micrograms of cotinine / g matrix, and at least about 3 micrograms of damascenone / g matrix. Alternatively or additionally, the aerosol preferably contains up to about 35 micrograms of neonicotinoid / g matrix, up to about 18 micrograms of cotinine / g matrix, and up to about 8 micrograms of damascenone / g matrix.
[0113] Nicotine may optionally be introduced into the aerosol-generating matrix, but for the purposes of this invention, it will be considered a non-tobacco material. Nicotine may comprise one or more nicotine salts selected from the following list: nicotine lactate, nicotine citrate, nicotine pyruvate, nicotine bitartrate, nicotine benzoate, nicotine pectate, nicotine alginate, and nicotine salicylate. Nicotine may be introduced in addition to tobacco having a low nicotine content, or it may be introduced into an aerosol-generating matrix having a reduced or zero tobacco content.
[0114] In some embodiments of the invention, the aerosol generating matrix comprises a homogenized rosemary material formed from granular plant material consisting only of rosemary particles, wherein nicotine, such as nicotine salts, is introduced into the aerosol generating matrix.
[0115] Preferably, the aerosol generating matrix comprises at least about 0.1 mg of nicotine per gram of matrix on a dry weight basis. More preferably, the aerosol generating matrix comprises at least about 0.5 mg of nicotine per gram of matrix on a dry weight basis, more preferably at least about 1 mg of nicotine per gram of matrix, more preferably at least about 1.5 mg of nicotine per gram of matrix, more preferably at least about 2 mg of nicotine per gram of matrix, more preferably at least about 3 mg of nicotine per gram of matrix, more preferably at least about 4 mg of nicotine per gram of matrix, and more preferably at least about 5 mg of nicotine per gram of matrix.
[0116] Preferably, the aerosol generating matrix comprises up to about 50 mg of nicotine per gram of matrix on a dry weight basis. More preferably, the aerosol generating matrix comprises up to about 45 mg of nicotine per gram of matrix on a dry weight basis, more preferably up to about 40 mg of nicotine per gram of matrix, more preferably up to about 35 mg of nicotine per gram of matrix, more preferably up to about 30 mg of nicotine per gram of matrix, more preferably up to about 25 mg of nicotine per gram of matrix, and more preferably up to about 20 mg of nicotine per gram of matrix on a dry weight basis.
[0117] For example, the aerosol generating matrix may contain about 0.1 mg to about 50 mg of nicotine per gram of matrix, or about 0.5 mg to about 45 mg of nicotine per gram of matrix, or about 1 mg to about 40 mg of nicotine per gram of matrix, or about 2 mg to about 35 mg of nicotine per gram of matrix, or about 5 mg to about 30 mg of nicotine per gram of matrix, or about 10 mg to about 25 mg of nicotine per gram of matrix, or about 15 mg to about 20 mg of nicotine per gram of matrix. In some preferred embodiments of the invention, the aerosol generating matrix contains about 1 mg to about 20 mg of nicotine per gram of matrix, based on dry weight.
[0118] The defined range of nicotine content in the aerosol generating matrix includes all forms of nicotine that may be present in the aerosol generating matrix, including nicotine inherent in tobacco materials and nicotine that has been optionally added separately to the aerosol generating matrix, for example, in the form of nicotine salts.
[0119] For example, the granular plant material may contain more preferably about 45% to about 60% by weight of tobacco particles, more preferably about 50% to about 65% by weight of tobacco particles on a dry weight basis.
[0120] In addition to rosemary pellets or a combination of rosemary pellets and tobacco pellets (“granular plant material”), homogenized rosemary material may also contain a certain proportion of other plant-flavored pellets.
[0121] For the purposes of this invention, the term "other plant-flavored particles" refers to particles of plant materials that are not rosemary, tobacco, or cannabis, which are capable of generating one or more flavorings upon heating. This term should be considered to exclude particles of inert plant materials such as cellulose, which do not contribute to the sensory output of the aerosol-generating matrix. The particles can be derived from ground or pulverized leaves, fruits, stems, stalks, roots, seeds, buds, or bark of other plants. Suitable plant-flavored particles included in the aerosol-generating matrix according to the invention will be known to those skilled in the art and include, but are not limited to, clove particles and tea particles.
[0122] By blending different plant particles of varying quantities and types, the composition of homogenized plant materials can be advantageously tuned. This allows for the formation of aerosol-generating matrices from a single homogenized plant material, if desired, without the need for combinations or mixing of different blends, as is the case, for example, in the production of conventional shredded fillers. Therefore, the production of aerosol-generating matrices can potentially be simplified.
[0123] The particulate plant material used in the aerosol-generating matrix of the present invention is adapted to provide a desired particle size distribution. Particle size distribution is expressed herein as a D-value, where the D-value refers to the percentage of particles with a diameter less than or equal to a given D-value. For example, in a D95 particle size distribution, 95% of the particles have a diameter less than or equal to a given D95 value, and 5% of the particles have a diameter greater than a given D95 value. Similarly, in a D5 particle size distribution, 5% of the particles have a diameter less than or equal to a D5 value, and 95% of the particles have a diameter greater than a given D5 value. The D5 and D95 values, combined, thus provide an indication of the particle size distribution of the particulate plant material.
[0124] Granular plant material can have a D95 value greater than or equal to 50 micrometers to less than or equal to 400 micrometers. This means that granular plant material can have a distribution represented by any D95 value within a given range, i.e., D95 can be equal to 50 micrometers, or D95 can be equal to 55 micrometers. etc. The range extends up to D95, which can be equal to 400 micrometers. By providing D95 values within this range, the inclusion of relatively large plant particles in the homogenized plant 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 homogenized plant materials can adversely affect the material's consistency.
[0125] Preferably, the granular plant material may have a D95 value greater than or equal to about 50 micrometers to less than or equal to about 350 micrometers, more preferably a D95 value greater than or equal to about 100 micrometers to less than or equal to about 300 micrometers. Both the granular rosemary material and the granular tobacco material may have a D95 value greater than or equal to about 50 micrometers to less than or equal to about 400 micrometers, preferably a D95 value greater than or equal to 100 micrometers to less than or equal to about 350 micrometers, more preferably a D95 value greater than or equal to about 200 micrometers to less than or equal to about 300 micrometers.
[0126] Preferably, the granular plant material may have a D5 value greater than or equal to about 10 micrometers to less than or equal to about 50 micrometers, more preferably a D5 value greater than or equal to about 20 micrometers to less than or equal to about 40 micrometers. By providing a D5 value within this range, very small dust particles will be avoided from being included in the homogenized rosemary material, which is likely desirable from a manufacturing perspective.
[0127] In some implementations, the granular plant material may be intentionally ground to form particles with a desired particle size distribution. Using intentionally ground plant material will advantageously improve the uniformity of the granular plant material and the consistency of the homogenized rosemary material.
[0128] The diameter of 100% granular plant material can be less than or equal to about 300 micrometers, more preferably less than or equal to about 250 micrometers. The diameter of 100% granular rosemary material and 100% granular tobacco material can be less than or equal to about 300 micrometers, more preferably less than or equal to about 250 micrometers. The particle size range of rosemary granules allows them to be combined with tobacco granules in existing cast leaf processes.
[0129] The homogenized rosemary material preferably comprises at least about 55% by weight, based on dry weight, of the granular plant material containing rosemary particles as described above, more preferably at least about 60% by weight, and even more preferably at least about 65% by weight. The homogenized rosemary material preferably comprises no more than about 95% by weight, based on dry weight, more preferably no more than about 90% by weight, and even more preferably no more than about 85% by weight. For example, the homogenized rosemary material may comprise about 55% to about 95% by weight, or about 60% to about 90% by weight, or about 65% to about 85% by weight, based on dry weight. In a particularly preferred embodiment, the homogenized rosemary material comprises about 75% by weight, based on dry weight.
[0130] Therefore, granular plant materials are often combined with one or more other components to form homogenized rosemary materials.
[0131] The homogenized rosemary material also includes a binder to modify the mechanical properties of the granular plant material, wherein the binder is included in the homogenized rosemary material during the manufacturing process 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; cellulose 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. Preferably, the binder comprises guar gum.
[0132] As defined above, the binder is present in an amount of about 1% to about 10% by weight based on the dry weight of the homogenized rosemary material, preferably in an amount of about 2% to about 5% by weight based on the dry weight of the homogenized rosemary material.
[0133] Additionally, the homogenized rosemary material may optionally contain one or more lipids to facilitate the diffusion of volatile components (e.g., aerosol forming agents, (E)-anesthelin, and nicotine), wherein said lipids are contained in the homogenized rosemary material during the manufacturing process as described herein. Suitable lipids contained in the homogenized rosemary material include, but are not limited to: medium-chain triglycerides, cocoa butter, palm oil, palm kernel oil, mango oil, 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.
[0134] Alternatively or additionally, homogenized rosemary materials may also contain pH adjusters.
[0135] Alternatively or additionally, the homogenized rosemary material may also contain fibers to modify the mechanical properties of the homogenized rosemary material, wherein said fibers are included in the homogenized rosemary material during the manufacturing process as described herein. Suitable exogenous fibers included in the homogenized rosemary material are those known in the art and include fibers formed from non-tobacco and non-rosemary materials, including but not limited to: cellulose fibers; cork fibers; hardwood fibers; jute fibers, and combinations thereof. Exogenous fibers derived from tobacco and / or rosemary may also be added. Any fibers added to the homogenized rosemary material are not considered part of the formation of “granular plant material” as defined above. Prior to being included in the homogenized rosemary material, the fibers may be treated 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.
[0136] Suitable fibers typically have a length greater than 400 micrometers 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 matrix. The amount of fiber in the homogenized rosemary material can depend on the type of material and, in particular, the method used to produce the homogenized rosemary material. In some embodiments, the fibers may be present in an amount of from about 2% to about 15% by weight, most preferably about 4% by weight, based on the dry weight of the matrix. This level of fiber may be present, for example, when the homogenized rosemary 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. This higher level of fiber is likely to be provided, for example, when the homogenized rosemary material is plant paper formed during a papermaking process.
[0137] As defined above, homogenized rosemary materials also contain one or more aerosol forming agents. During volatilization, aerosol forming agents can transport other volatile compounds, such as nicotine and flavorings, released from the aerosol-generating matrix upon heating within the aerosol. The aerosolization of specific compounds from the aerosol-generating matrix is not determined solely by their boiling point. The amount of aerosolized compounds can be influenced by the physical form of the matrix and other components also present in the matrix. The stability of compounds within the temperature and time range of aerosolization will also affect the amount of compounds present in the aerosol.
[0138] Suitable aerosol forming agents included in homogenized rosemary materials are known in the art and include, but are not limited to: polyols such as triethylene glycol, propylene glycol, 1,3-butanediol, and glycerol; esters of polyols such as glycerol monoacetate, glycerol diacetate, or glycerol triacetate; and aliphatic esters of mono-, di-, or polycarboxylic acids such as dimethyl dodecanoate and dimethyl tetradecanoate. Homogenized rosemary materials may contain a single aerosol forming agent or a combination of two or more aerosol forming agents.
[0139] The homogenized rosemary material has an aerosol forming agent content of about 5% to about 30% by weight, about 10% to about 25% by weight, or about 15% to about 20% by weight, based on dry weight.
[0140] For example, if the matrix is intended for use in an aerosol-generating article of an electrically operated aerosol-generating system with a heating element, it may preferably contain an aerosol-forming agent content of about 5% to about 30% by weight on a dry weight basis. If the matrix is intended for use in an aerosol-generating article of an electrically operated aerosol-generating system with a heating element, the aerosol-forming agent is preferably glycerol.
[0141] In other embodiments, the homogenized rosemary 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 matrix is intended for use in an aerosol-generating article in which the aerosol forming agent is held in a reservoir separate from the matrix, the matrix may have an aerosol forming agent content greater than 1% and less than about 5%. In such embodiments, the aerosol forming agent volatilizes upon heating, and the flow of the aerosol forming agent contacts the aerosol-generating matrix to entrain flavor compounds from the aerosol-generating matrix in the aerosol.
[0142] Aerosol forming agents can act as wetting agents in aerosol generation matrices.
[0143] Alternatively or additionally, the homogenized rosemary material may also contain an acid. The acid may contain a carboxylic acid. The carboxylic acid may contain a ketone group. Preferably, the carboxylic acid may contain a ketone group having less than about 10 carbon atoms, or less than about 6 carbon atoms, or less than about 4 carbon atoms, such as levulinic acid or lactic acid. As described below, the inclusion of an acid may be particularly advantageous when the aerosol-forming matrix is in gel form.
[0144] The homogenized plant material of the aerosol-generating matrix according to the present invention may comprise a single type of homogenized plant material or two or more types of homogenized plant materials having different compositions or forms. For example, in one embodiment, the aerosol-generating matrix comprises rosemary particles and tobacco particles contained within the same sheet of homogenized plant material. However, in other embodiments, the aerosol-generating matrix may contain tobacco particles and rosemary particles within separate sheets.
[0145] The homogenized rosemary material is preferably in solid or gel form. However, in some embodiments, the homogenized material may be in a solid form that is not a gel. Preferably, the homogenized rosemary material is not in the form of a film.
[0146] Homogenized rosemary material can be provided in any suitable form. For example, homogenized rosemary material can be in the form of one or more sheets. As used herein in conjunction with the invention, the term "sheet" describes a layered element whose width and length are much greater than its thickness.
[0147] Alternatively or otherwise, homogenized rosemary material may be in the form of multiple pellets or granules.
[0148] Alternatively or additionally, the homogenized rosemary material may be in the form of a fillable tube or hookah consumable, or in a form suitable for use in hookah devices. The present invention includes tubes or hookah devices containing homogenized rosemary material.
[0149] Alternatively or additionally, homogenized rosemary material may be in the form of multiple strips, bars, or fragments. As used herein, the term "strip" describes an elongated material element whose length is much greater than its width and thickness. The term "strip" should be considered to encompass bars, fragments, and any other homogenized rosemary material of similar form. Strips of homogenized rosemary material may be formed from sheets of homogenized rosemary material, for example by cutting or shredding, or by other methods, such as extrusion.
[0150] In some embodiments, due to the splitting or cracking of the homogenized rosemary material sheet during the formation of the aerosol-generating matrix, for example due to compression, thin strips can be formed within the aerosol-generating matrix. In situ Formation. The homogenized rosemary material strips within the aerosol-generating matrix can be separated from each other. Alternatively, each strip of homogenized rosemary material within the aerosol-generating matrix can be at least partially connected to one or more adjacent strips along its length. For example, adjacent strips can be connected by one or more fibers. This can occur, for example, due to the splitting of the homogenized rosemary material sheet during the production of the aerosol-generating matrix as described above.
[0151] Preferably, the aerosol generating matrix is in the form of one or more sheets of homogenized rosemary material. In various embodiments of the invention, the one or more sheets of homogenized rosemary material can be produced by a casting process. In various embodiments of the invention, the one or more sheets of homogenized rosemary material can be produced by a papermaking process. The one or more sheets described herein may each individually have a thickness of 100 micrometers to 600 micrometers, preferably 150 micrometers to 300 micrometers, and most preferably 200 micrometers to 250 micrometers. Individual thickness refers to the thickness of a single sheet, while combined thickness refers to the total thickness of all sheets constituting the aerosol generating matrix. For example, if the aerosol generating matrix is formed from two separate sheets, the combined thickness is the sum of the thicknesses of the two separate sheets, or, in the case of two sheets stacked in the aerosol generating matrix, the measured thickness of the two sheets.
[0152] One or more sheets as described herein may each individually have approximately 100 g / m³ 2 Approximately 300g / m 2 The weight per square meter.
[0153] One or more sheets as described herein may each individually have approximately 0.3 g / cm³. 3 Approximately 1.3 g / cm³ 3 Preferably, it is about 0.7 g / cm³. 3 To approximately 1.0 g / cm 3 The density.
[0154] The term "tensile strength" is used throughout this specification to describe the force required to stretch a sheet of homogenized rosemary 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 it is measured in either the longitudinal or transverse direction of the sheet material. The unit of tensile strength is Newtons per meter (N / m). Methods for measuring the tensile strength of sheets are well-known. A suitable test description is found 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".
[0155] The materials and equipment required for testing according to ISO 1924-2 are: a general-purpose tensile / compression testing machine, Instron 5566, or equivalent; a 100-Newton tension load cell, Instron, or equivalent; two pneumatic clamps; a steel gauge block 180 ± 0.25 mm long (approximately 10 mm wide and 3 mm thick); a double-blade strip cutter, 15 ± 0.05 × approximately 250 mm, Adamel Lhomargy, or equivalent; a scalpel; a computer running Merlin acquisition software, or equivalent; and compressed air.
[0156] Samples were prepared by first conditioning homogenized rosemary material sheets at 22±2 degrees Celsius and 60±5% relative humidity for at least 24 hours before testing. The samples were then cut longitudinally or transversely to approximately 250 × 15±0.1 mm using a double-blade slicer. The edges of the specimens must be cut cleanly and precisely; therefore, no more than three specimens should be cut simultaneously.
[0157] The tensile / compression testing instrument was set up by installing a 100-Newton tension load sensor, connecting a general-purpose tensile / compression testing machine and a computer, and selecting a pre-defined measurement method in the software, with the test speed set to 8 mm per minute. The tension load sensor was then calibrated and pneumatic clamps were installed. The test distance between the pneumatic clamps was adjusted to 180 ± 0.5 mm using steel gauge blocks, and both the distance and force were set to zero.
[0158] The sample is then placed upright in the center between the clamps, avoiding touching the test area with fingers. The upper clamp is closed, and the paper strip is suspended in the open lower clamp. The force is set to zero. Then, the paper strip is gently pulled down to close the lower clamp; the initial force must be between 0.05 and 0.20 Newtons. As the upper clamp moves upward, a gradually increasing force is applied until the sample breaks. The same procedure is repeated for the remaining samples. A result is valid when the sample breaks when the clamps are separated by a distance greater than 10 mm. If this is not the case, the result is rejected, and additional measurements are performed.
[0159] When the available test specimens of homogenized rosemary material are smaller than those described above in the test according to ISO 1924-2, the test can be easily scaled down to accommodate the available test specimen size.
[0160] One or more sheets of the homogenized rosemary material described herein may each individually have a peak tensile strength of 50 N / m to 400 N / m in the transverse direction, or preferably 150 N / m to 350 N / m. Considering that sheet thickness affects tensile strength, and given that a batch of sheets may exhibit thickness variations, it may be desirable to normalize this value to a specific sheet thickness.
[0161] One or more sheets as described herein may each individually have a peak tensile strength of 100 N / m to 800 N / m, or preferably 280 N / m to 620 N / m, in the longitudinal direction, normalized to a sheet thickness of 215 μm. The longitudinal direction refers to the direction in which the sheet material will be wound onto or unwound from a spool and fed into the machine, while the transverse direction is perpendicular to the longitudinal direction. This tensile strength value makes the sheets and methods described herein particularly suitable for subsequent operations involving mechanical stress.
[0162] Providing sheets with the thickness, weight per square meter, and tensile strength levels defined above will advantageously optimize the sheet's machinability to form an aerosol-generating matrix and ensure that damage, such as tearing, is avoided during high-speed processing of the sheet.
[0163] In embodiments of the invention in which the aerosol-generating matrix comprises one or more sheets of homogenized rosemary material, the sheets are preferably in the form of one or more aggregated sheets. As used herein, the term “aggregate” means that the homogenized rosemary material sheet is wound, folded, or otherwise compressed or contracted into a cylindrical shape substantially transverse to the axis of the rod or strip. The step of “aggregating” the sheet can be performed by any suitable device that provides the necessary transverse compression of the sheet.
[0164] As used herein, the term "longitudinal" refers to the direction corresponding to the main longitudinal axis of the aerosol-generating article extending between its upstream and downstream ends. During use, air is drawn through the aerosol-generating article in the longitudinal direction. The term "transverse" refers to the 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 bar with a circular cross-section, the maximum width corresponds to the diameter of the circle.
[0165] As used herein, the term "bar" 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 may be greater than or equal to the length of a bar. Typically, the length of a strip is greater than the length of a bar. A strip may comprise one or more bars, preferably aligned longitudinally.
[0166] As used herein, the terms “upstream” and “downstream” describe the relative position of an element or portion of an aerosol-generating article with respect to the direction in which the aerosol is delivered through the aerosol-generating article during use. The downstream end of the airflow path is the end where the aerosol is delivered to the user of the article.
[0167] One or more sheets of homogenized rosemary material may be aggregated laterally relative to its longitudinal axis and wrapped with packaging to form continuous strips or bars. The continuous strips may be cut into multiple discrete strips or bars. The packaging may be paper or non-paper, as described in more detail below.
[0168] Alternatively, one or more sheets of homogenized rosemary material can be cut into strips as described above. In such embodiments, the aerosol-generating matrix comprises a plurality of homogenized rosemary material strips. These 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.
[0169] The length of the strips is preferably greater than about 5 mm, for example, between about 5 mm and about 15 mm, about 8 mm and about 12 mm, or about 12 mm. Preferably, the strips have substantially the same length as each other. The length of the strips can be determined by the manufacturing process, thereby cutting the strips into shorter bars, and the length of the strips corresponds to the length of the bars. The strips may be fragile, which may lead to breakage, especially during transportation. In this case, some strips may be shorter than the length of the bars.
[0170] The plurality of strips preferably extend substantially longitudinally, aligned with the longitudinal axis along the length of the aerosol-generating matrix. Preferably, the plurality of strips are thus aligned substantially parallel to each other. The plurality of longitudinal strips of the aerosol-generating material are preferably substantially non-curled.
[0171] The homogenized rosemary material strips preferably each have a mass-to-surface-area ratio of at least about 0.02 mg / mm², more preferably at least about 0.05 mg / mm². Preferably, the homogenized rosemary material strips each have a mass-to-surface-area ratio of no more than about 0.2 mg / mm², more preferably no more than about 0.15 mg / mm². The mass-to-surface-area ratio is calculated by dividing the mass of the homogenized rosemary material strips in millimeters by the geometric surface area of the homogenized rosemary material strips in millimeters.
[0172] One or more sheets of homogenized rosemary material can be textured by crimping, embossing, or perforation. The texture can be applied to one or more sheets before aggregation or before being cut into strips. Preferably, one or more sheets of homogenized rosemary material are crimped before aggregation, such that the homogenized rosemary material is in the form of crimped sheets, more preferably in the form of aggregated crimped sheets. As used herein, the term "crimped sheet" refers to a sheet having a plurality of substantially parallel ridges or corrugations generally aligned with the longitudinal axis of the article.
[0173] In one embodiment, the aerosol generating matrix may be in the form of a single rod of the aerosol generating matrix. Preferably, the rod of the aerosol generating matrix may comprise multiple strips of homogenized rosemary material. Most preferably, the rod of the aerosol generating matrix may comprise one or more sheets of homogenized rosemary material. Preferably, the one or more sheets of homogenized rosemary material may be press-fitted, such that they have multiple ridges or corrugations substantially parallel to the cylindrical axis of the rod. This process will advantageously promote the aggregation of the press-fitted sheets of homogenized rosemary material to form the rod. Preferably, one or more sheets of homogenized rosemary material may be aggregated. It should be understood that the press-fitted sheets of homogenized rosemary material may alternatively or additionally have multiple substantially parallel ridges or corrugations arranged at acute or obtuse angles to the cylindrical axis of the rod. The sheets may be pressed to such an extent that the integrity of the sheets is compromised at the multiple parallel ridges or corrugations, causing material separation and resulting in the formation of fragments, strips, or slivers of homogenized rosemary material.
[0174] In another embodiment, the aerosol-generating matrix comprises a first rod and a second rod, the first rod comprising a first homogenized plant material and the second rod comprising a second homogenized plant material, wherein the first homogenized plant material and the second homogenized plant material comprise different levels of rosemary particles and tobacco particles. At least one of the first homogenized plant material and the second homogenized plant material is homogenized rosemary material. For example, the first homogenized plant material may comprise about 1% to about 25% by weight of rosemary particles on a dry weight basis; while the second homogenized plant material may comprise 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 matrix comprises at least 2.5% by weight of rosemary particles and up to 70% by weight of tobacco particles on a dry weight basis.
[0175] In this arrangement, the first homogenized plant material preferably comprises a first granular plant material with a higher proportion of rosemary particles than the second homogenized plant material. The second homogenized plant material may be homogenized tobacco material, which is substantially free of rosemary particles.
[0176] Preferably, the first homogenized plant material may be in the form of one or more sheets, and the second homogenized plant material may be in the form of one or more sheets.
[0177] Optionally, the aerosol-generating matrix may comprise one or more rods. Preferably, the matrix may comprise a first rod and a second rod, wherein a first homogenized plant material may be located in the first rod, and a second homogenized plant material may be located in the second rod.
[0178] Two or more bars can be combined and extended in an adjacent end-to-end relationship to form a strip. Two bars can be placed longitudinally with a gap between them, thereby creating a cavity within the strip. The bars can be arranged in any suitable manner within the strip.
[0179] For example, in a preferred arrangement, a downstream bar containing a predominant proportion of rosemary particles may be adjacent to an upstream bar containing a predominant proportion of tobacco particles to form a bar. Alternative configurations in which the upstream and downstream positions of the respective bars change relative to each other are also contemplated. Alternative configurations in which a third homogenized plant material containing different proportions of rosemary particles and tobacco particles forms a third bar are also contemplated. When two or more bars are provided, the homogenized plant material may be provided in the same form in each bar, or in different forms in each bar, i.e., aggregated or shredded. Optionally, one or more bars may be individually or together wrapped in a thermally conductive sheet material, as described below.
[0180] The first rod may contain one or more sheets of a first homogenized plant material, and the second rod may contain one or more sheets of a second homogenized plant material. The total length of the rods may be between about 10 mm and about 40 mm, preferably between about 10 mm and about 15 mm, more preferably about 12 mm. The first and second rods may have the same length or may have different lengths. If the first and second rods have the same length, the length of each rod may preferably be between about 6 mm and about 20 mm. Preferably, the second rod may be longer than the first rod to provide a desired ratio of tobacco particles to rosemary particles in the matrix. In summary, the matrix preferably contains 0% to 75% by weight of tobacco particles and 25% to 1% by weight of rosemary particles on a dry weight basis. Preferably, the second rod is at least 40% to 50% longer than the first rod.
[0181] If the first homogenized plant material and the second homogenized plant material are in the form of one or more sheets, then 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-fit sheets. It should be understood that all other physical properties described with reference to embodiments in which a single homogenized plant material is present also apply to embodiments in which both the first homogenized plant material and the second homogenized plant material are present. Furthermore, it should be understood that the description of additives (e.g., binders, lipids, fibers, aerosol forming agents, humectants, plasticizers, flavoring agents, fillers, aqueous and non-aqueous solvents, and combinations thereof) with reference to embodiments in which a single homogenized plant material is present also applies to embodiments in which both the first homogenized plant material and the second homogenized plant material are present.
[0182] In another embodiment of the aerosol-generating matrix, the first homogenized plant material is in the form of a first sheet, the second homogenized plant material is in the form of a second sheet, and the second sheet at least partially covers the first sheet.
[0183] The first sheet can be a textured sheet, and the second sheet can be untextured.
[0184] Both the first and second sheets can be textured sheets.
[0185] The first sheet can be a textured sheet that is textured in a different way 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.
[0186] Both the first and second sheets can be crimped sheets that differ in shape from each other. For example, compared to the first sheet, the second sheet can be crimped with a different amount of material per unit width.
[0187] These sheets can be assembled to form rods. The sheets assembled to form rods can have different physical dimensions. The width and thickness of the sheets can vary.
[0188] It may be necessary to aggregate two sheets together, each with a different thickness or width. This could alter the physical properties of the rod. This could facilitate the formation of aerosol-generating matrix blends of sheets with different chemical compositions.
[0189] The first sheet can have a first thickness, and the second sheet can have a second thickness, which is a multiple of the first thickness. For example, the second sheet can have a thickness that is two or three times that of the first sheet.
[0190] The first sheet may have a first width, and the second sheet may have a second width different from the first width.
[0191] The first and second sheets can be arranged in an overlapping relationship before being joined together or at the point where they are joined. These sheets can have the same width and thickness. These sheets can have different thicknesses. These sheets can have different widths. The sheets can have different textures.
[0192] When it is desired that both the first and second sheets be textured, the sheets can be textured simultaneously before aggregation. For example, the sheets can be overlapped and passed through a texturing device, such as a pair of pressing rollers. (Refer to WO-A-2013 / 178766) Figure 2Suitable equipment and methods for simultaneous pressing are described. In a preferred embodiment, a second sheet of second homogenized plant material covers a first sheet of first homogenized plant material, and the combined sheets are aggregated to form a rod of aerosol-generating matrix. Optionally, the sheets can be pressed together prior to aggregation to facilitate aggregation.
[0193] Alternatively, each sheet can be textured separately and then put together to form a rod. For example, in the case where the two sheets have different thicknesses, it may be desirable to press the first sheet differently relative to the second sheet.
[0194] It should be understood that all other physical properties described with reference to embodiments containing a single homogenized rosemary material also apply to embodiments containing a first homogenized plant material and a second homogenized plant material. Furthermore, it should be understood that descriptions of additives (e.g., binders, lipids, fibers, aerosol forming agents, humectants, plasticizers, flavoring agents, fillers, aqueous and non-aqueous solvents, and combinations thereof) with reference to embodiments containing a single homogenized rosemary material also apply to embodiments containing both a first homogenized plant material and a second homogenized plant material.
[0195] The homogenized rosemary material used in the aerosol generation matrix according to the present invention can be produced by various methods, including papermaking, casting, dough reconstitution, extrusion or any other suitable process.
[0196] Preferably, the homogenized rosemary material is in the form of a “cast leaf.” The term “cast leaf” is used herein to refer to a sheet product obtained by a casting process, which is based on casting a slurry containing plant particles (e.g., rosemary particles or a mixture of tobacco particles and rosemary particles) and a binder (e.g., guar gum) onto a support surface such as a belt conveyor, drying the slurry, and removing the dried sheet from the support surface. Examples of casting or cast leaf processes are described, for example, in US-A-5,724,998, for the manufacture of cast leaf tobacco. In the cast leaf process, granular plant material is mixed with a liquid component (typically water) to form a slurry. Other additives in the slurry may include fibers, binders, and aerosol-forming agents. The granular plant material may agglomerate in the presence of a binder. The slurry is cast onto a support surface and dried to form a sheet of homogenized rosemary material.
[0197] In some preferred embodiments, the homogenized rosemary material used in the articles according to the invention is produced by casting. Homogenized rosemary materials prepared by casting typically comprise agglomerated granular plant material.
[0198] In the cast leaf process, because virtually all soluble fractions are retained in the plant material, most of the flavor is advantageously preserved. Additionally, energy-intensive papermaking steps are avoided.
[0199] In a preferred embodiment of the invention, to form a homogenized rosemary material, a mixture comprising particulate plant material, water, a binder, and an aerosol forming agent is formed. Both the particulate plant material and the aerosol forming agent are as described above, referring to the first aspect of the invention. A sheet is formed from this mixture, and then the sheet is dried. Preferably, the mixture is an aqueous mixture. As used herein, "dry weight" refers to the weight, expressed as a percentage, of a specific non-aqueous component relative to the total weight of all non-aqueous components in the mixture. The composition of an aqueous mixture can be expressed as "dry weight percentage." This refers to the weight, expressed as a percentage, of the non-aqueous component relative to the entire aqueous mixture.
[0200] The mixture can be a slurry. As used herein, a "slurry" is a homogenized aqueous mixture with a relatively low dry weight. The slurry used in this method preferably has a dry weight of 5% to 60%.
[0201] Alternatively, the mixture may be agglomerates. As used herein, a "gglomerate" is an aqueous mixture having a relatively high dry weight. Agglomerates used in the methods herein preferably have a dry weight of at least 60%, more preferably at least 70%.
[0202] In some embodiments of the method of the present invention, it is preferred to include a slurry and lumps with a dry weight of more than 30%.
[0203] The step of mixing granular plant material, water, and other optional components can be carried out by any suitable method. For low-viscosity mixtures, i.e., some slurries, high-energy mixers or high-shear mixers are preferred. This mixing breaks down and homogenizes the phases of the mixture. For higher-viscosity mixtures, i.e., some lumps, kneading methods can be used to homogenize the various phases of the mixture.
[0204] The method according to the invention may further include the step of vibrating the mixture to distribute the various components. Vibrating the mixture, i.e., vibrating a tank or silo containing a homogenized mixture, can help homogenize the mixture, especially when the mixture is a low-viscosity mixture, i.e., some slurry. If vibration and mixing are performed, less mixing time may be required to homogenize the mixture to the target value optimal for casting.
[0205] If the mixture is a slurry, it is preferable to form a web of homogenized rosemary material using a casting process, which includes casting the slurry on a support surface such as a belt conveyor. A method for producing homogenized rosemary 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. The sheet can then be removed from the support surface after drying. The cast sheet has tensile strength, allowing it to be mechanically manipulated and unwound from a roll without breaking or deforming.
[0206] If the mixture is in the form of lumps, the lumps can be extruded as sheets, strips, or bars before the drying and extrusion step. Preferably, the lumps can be extruded as sheets. The extruded mixture can be dried at room temperature or at a 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 extruded mixture after drying is between about 5% and about 15% based on the total weight of the sheet. Sheets formed from lumps require less drying time and / or lower drying temperatures because the moisture content is significantly lower compared to webs formed from slurry.
[0207] After the sheet is dried, the method may optionally include the step of coating the sheet with nicotine salt, preferably together with an aerosol forming agent, as described in WO-A-2015 / 082652.
[0208] After the sheet has dried, the method according to the invention may optionally include the step of cutting the sheet into strips, fragments, or strips for forming the aerosol generating matrix as described above. Suitable means may be used to assemble the strips, fragments, or strips together to form strips of the aerosol generating matrix. In the formed strips of the aerosol generating matrix, 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.
[0209] The method according to the invention may optionally include a step of winding the sheet onto a roll after the drying step.
[0210] The present invention also provides an alternative papermaking method for producing homogenized plant material sheets in the form of "plant paper".
[0211] Plant paper refers to reconstituted plant sheets formed by a method in which plant raw materials are extracted with solvents to produce extracts of soluble plant compounds and insoluble residues of fibrous plant materials, and the extracts and insoluble residues are then recombined. The extracts may optionally be concentrated or further processed before being recombined with the insoluble residues. The insoluble residues may optionally be refined and combined with additional plant fibers before being recombined with the extracts. In the method according to the invention, the plant raw materials will comprise rosemary granules, optionally combined with tobacco granules.
[0212] More specifically, the method for producing plant paper includes a first step of mixing plant material with water to form a dilute suspension. The dilute suspension primarily consists of individual cellulose fibers. The suspension has a lower viscosity and a higher water content compared to the slurry produced in a casting process. This first step may include soaking, optionally in the presence of an alkali such as sodium hydroxide, and optionally with the application of heat.
[0213] The method further includes a second step of separating the suspension into an insoluble portion containing insoluble residues of fibrous plant material and a liquid or aqueous extract containing soluble plant compounds. Water remaining in the insoluble residues of the fibrous plant material can be drained through a screen acting as a sieve, allowing a web of randomly interwoven fibers to be laid out. Water can be further removed from this web by pressing with rollers, sometimes with suction or vacuum assistance.
[0214] After removing the aqueous portion and water, the insoluble residue forms a sheet. Preferably, a generally flat and uniform plant fiber sheet is formed.
[0215] Preferably, the method further includes the steps of concentrating an extract of soluble plant compounds removed from the sheet and adding the concentrated extract to a sheet of insoluble fibrous plant material to form a sheet of homogenized plant material. Alternatively or additionally, soluble plant material or concentrated plant material from another method 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.
[0216] As described in US-A-3,860,012, this process has been used with tobacco to manufacture reconstituted tobacco products, also known as tobacco paper. The same method can also be used with one or more plants to produce sheet materials of paper-like textures, such as sheets of rosemary paper.
[0217] In some preferred embodiments, the homogenized rosemary material used in the articles according to the invention is produced by a papermaking process as defined above. The homogenized tobacco material or homogenized rosemary material produced by such a process is referred to as tobacco paper or rosemary paper. Homogenized plant materials produced by the papermaking process can be distinguished by the large number of fibers present throughout the material, visible to the naked eye or under an optical microscope, particularly when the paper is wetted. In contrast, homogenized plant materials produced by the casting process contain fewer fibers than paper and tend to dissociate into a pulp when wetted. Blended tobacco rosemary paper refers to homogenized plant material produced by this method using a mixture of tobacco and rosemary materials.
[0218] In embodiments where the aerosol-generating matrix comprises a combination of rosemary particles and tobacco particles, the aerosol-generating matrix may comprise one or more sheets of rosemary paper and one or more sheets of tobacco paper. The rosemary paper and tobacco paper sheets may be interlaced or stacked before being aggregated to form a strip. Optionally, the sheets may be crimped. Alternatively, the rosemary paper and tobacco paper sheets may be cut into strips, bars, or fragments and then assembled to form a strip. The relative amounts of tobacco and rosemary in the aerosol-generating matrix can be adjusted by varying the respective numbers of tobacco and rosemary sheets or the respective amounts of rosemary and tobacco strips, bars, or fragments in the strip.
[0219] For example, the quantity or amount of tobacco and rosemary sheets or strips can be adjusted to provide a rosemary to tobacco ratio of approximately 1:4, 1:9, or 1:30.
[0220] Other known processes applicable to the production of homogenized plant materials are, for example, agglomeration processes of the type described in US-A-3,894,544; and extrusion processes of the type described in GB-A-983,928. Generally, the density of homogenized plant materials produced by extrusion and agglomeration processes is greater than that produced by casting processes.
[0221] In an alternative embodiment of the invention, the homogenized rosemary material is in the form of a gel composition formed from rosemary particles, an aerosol forming agent, and a binder.
[0222] Preferably, when the homogenized rosemary material is in the form of a gel composition containing rosemary particles, the binder comprises a cellulose ether such as carboxymethyl cellulose. The binder may be present in an amount of about 1% to about 5% by weight based on the total weight of the gel. For example, the gel composition may contain 1.5% to 3.5% by weight of sodium carboxymethyl cellulose.
[0223] Preferably, the gel composition contains at least about 60% by weight of an aerosol-forming agent such as glycerol based on the total weight of the gel. For example, the gel composition may contain 65% to 85% by weight of glycerol.
[0224] Optionally, the gel composition may also contain an acid, such as lactic acid. The acid may be present in an amount of up to about 6% by weight based on the total weight of the gel composition. Optionally, the gel composition may contain up to about 5% by weight of nicotine based on the total weight of the gel composition. Optionally, the gel composition contains about 10% to about 30% by weight of water based on the total weight of the gel composition.
[0225] In embodiments where the homogenized rosemary material is in the form of a gel composition, the aerosol-generating matrix preferably comprises a porous medium loaded with the gel composition. The term "porous" is used herein to refer to a material providing multiple pores or openings that allow air to pass through it.
[0226] The porous medium can be any suitable porous material capable of containing or retaining the gel composition. Ideally, the porous medium allows the gel composition to move within it. In certain embodiments, the porous medium comprises natural, synthetic, or semi-synthetic materials, or combinations thereof. In certain embodiments, the porous medium comprises sheet materials, foams, or fibers, such as loose fibers; or combinations thereof. In certain embodiments, the porous medium comprises woven, nonwoven, or extruded materials, or combinations thereof. Preferably, the porous medium comprises cotton, paper, viscose fibers, PLA, or cellulose acetate, or combinations thereof. Preferably, the porous medium comprises sheet materials, such as cotton or cellulose acetate. In a particularly preferred embodiment, the porous medium comprises a sheet made of cotton fibers.
[0227] The porous medium used in this invention can be either press-fitted or shredded. In a preferred embodiment, the porous medium is press-fitted. In an alternative embodiment, the porous medium comprises shredded porous medium. The pressing or shredding process can be performed before or after loading the gel composition.
[0228] Preferably, when the homogenized rosemary material is in the form of a gel composition loaded onto a porous medium, the aerosol-generating matrix comprises elongated receptor elements extending longitudinally through or adjacent to the porous medium.
[0229] Preferably, the aerosol generating matrix of the aerosol generating article according to the present invention contains at least about 200 mg of homogenized rosemary material, more preferably at least about 250 mg of homogenized rosemary material, and even more preferably at least about 300 mg of homogenized rosemary material.
[0230] The aerosol generating article according to the invention comprises a strip, said strip containing a matrix in one or more rods. The strip of aerosol generating matrix 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.
[0231] 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 the aerosol-generating matrix, the rod has the same length as the strip.
[0232] Depending on their intended use, the strips of the aerosol generating matrix can have an outer diameter of about 5 mm to about 10 mm. For example, in some embodiments, the strips can 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 the aerosol generating matrix corresponds to the diameter of the strip, including any packaging material.
[0233] The aerosol-generating matrix of the aerosol-generating article according to the invention preferably has at least a portion of its length surrounded by one or more packaging materials. The one or more packaging materials may include paper packaging materials, non-paper packaging materials, or both. Suitable paper packaging materials for specific embodiments of the invention are known in the art and include, but are not limited to: cigarette paper; and filter tip packaging materials. Suitable non-paper packaging materials for specific embodiments of the invention are known in the art and include, but are not limited to, sheets of homogenized tobacco material. Homogenized tobacco packaging materials are particularly suitable for embodiments in which the aerosol-generating matrix comprises one or more sheets of homogenized rosemary material formed from granular plant material, said granular plant material containing a combination of rosemary granules and a low weight percentage of tobacco granules, such as 20% to 0% tobacco granules by dry weight.
[0234] In some embodiments of the invention, at least a portion of the aerosol-generating matrix along its length is surrounded by a thermally conductive sheet material, such as metal foil (e.g., aluminum foil) or metallized paper. The metal foil or metallized paper serves to facilitate rapid heat conduction throughout the aerosol-generating matrix. Additionally, the metal foil or metallized paper can be used to prevent ignition of the aerosol-generating matrix in the event of a consumer attempting to ignite it. Furthermore, during use, the metal foil or metallized paper prevents odors generated when the outer packaging is heated from entering the aerosol generated by the aerosol-generating matrix. This may be a problem, for example, for aerosol-generating articles having an aerosol-generating matrix that is externally heated during use to generate aerosols. Alternatively or additionally, metallized packaging can be used to facilitate the detection or identification of the aerosol-generating article when it is inserted into an aerosol-generating device during use. The metal foil or metallized paper may contain metal particles, such as iron particles.
[0235] One or more packages surrounding the aerosol generating matrix preferably have a total thickness of about 0.1 mm to about 0.9 mm.
[0236] The inner diameter of the aerosol generating matrix strip 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" refers to the diameter of the aerosol generating matrix strip, excluding the thickness of the packaging, but the packaging is still in place when measured.
[0237] Aerosol-generating products according to the present invention also include, but are not limited to, tobacco cartridges or hookah consumables.
[0238] The aerosol generating article according to the invention may optionally include a support element comprising at least one hollow tube immediately downstream of the aerosol generating matrix. One function of the tube is to position the aerosol generating matrix toward a distal end of the aerosol generating article, such that the aerosol generating matrix can contact a heating element. When the heating element is inserted into the aerosol generating matrix, the tube serves to prevent the aerosol generating matrix from being forced along the aerosol generating article toward other downstream elements. The tube also acts as a spacer element to separate downstream elements from the aerosol generating matrix. The tube may be made of any material, such as cellulose acetate, polymer, cardboard, or paper.
[0239] Alternatively or additionally, the aerosol generating article according to the invention may optionally include an aerosol cooling element downstream of the aerosol generating matrix and immediately downstream of the hollow tube forming the support element. In use, the aerosol formed by volatile compounds released from the aerosol generating matrix passes through and is cooled by the aerosol cooling element before being inhaled by the user. The lower temperature allows vapor to condense into aerosol. The aerosol cooling element may be a hollow tube, such as a hollow cellulose acetate tube or a cardboard tube, which may resemble the support element immediately downstream of the aerosol generating matrix. The aerosol cooling element may be a hollow tube with an outer diameter equal to that of the hollow tube of the support element but with an inner diameter smaller or larger than that of the hollow tube of the support element.
[0240] In one embodiment, the aerosol cooling element encased in paper comprises 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 paperboard. In some embodiments, the aerosol cooling element encased in paper may comprise one or more sheets made of materials selected from 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 nonwoven filaments of materials selected from 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 press-fitted and aggregated sheet of polylactic acid encased in filter paper. In another preferred embodiment, the aerosol cooling element includes longitudinal channels and is made of woven filaments of synthetic polymers, such as polylactic acid filaments, which are wrapped in paper.
[0241] One or more additional hollow tubes may be provided downstream of the aerosol cooling element.
[0242] The aerosol generating article according to the invention may further include a filter or nozzle downstream of the aerosol generating matrix and, when present, a support element and an aerosol cooling element. The filter may contain one or more filter materials to remove particulate components, gaseous components, or combinations 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, zeolite, molecular sieves, and silica gel; biodegradable polymers, including, for example, polylactic acid (PLA), Mater-Bi®, hydrophobic viscose fibers, and bioplastics; and combinations thereof. The filter may be located downstream of the aerosol generating article. The filter may be a cellulose acetate filter nozzle segment. In one embodiment, the filter is about 7 mm long, but may have a length between about 5 mm and about 10 mm.
[0243] The aerosol-generating article according to the invention may include a mouth cavity at its downstream end. The mouth cavity may be defined by one or more packages extending downstream from a filter or mouthpiece. Alternatively, the mouth cavity may be defined by a separate tubular element disposed at the downstream end of the aerosol-generating article.
[0244] The aerosol generating article according to the invention preferably further includes a ventilation zone disposed along the position of the aerosol generating article. For example, the aerosol generating article may be disposed along a hollow tube downstream of the aerosol generating matrix.
[0245] The aerosol generating article according to the invention may optionally also include an upstream element at the upstream end of the aerosol generating matrix. The upstream element may be a porous rod element, such as a rod of fibrous filter material such as cellulose acetate.
[0246] In a preferred embodiment of the invention, the aerosol generating article comprises an aerosol generating matrix, at least one hollow tube downstream of the aerosol generating matrix, and a filter downstream of the at least one hollow tube. Optionally, the aerosol generating article further comprises an end cavity at the downstream end of the filter. Optionally, the aerosol generating article further comprises an upstream element at the upstream end of the aerosol generating matrix. Preferably, a ventilation zone is provided along the at least one hollow tube.
[0247] In a particularly preferred embodiment having this arrangement, the aerosol generating article comprises an aerosol generating matrix, an upstream element at an upstream end of the aerosol generating matrix, a support element downstream of the aerosol generating matrix, an aerosol cooling element downstream of the support element, and a filter downstream of the aerosol cooling element. Preferably, both the support element and the aerosol cooling element are in the form of hollow tubes. Preferably, the aerosol generating matrix includes elongated receptor elements extending longitudinally therethrough.
[0248] In a particularly preferred embodiment, the aerosol generating matrix has a length of about 33 mm and an outer diameter of about 5.5 mm to 6.7 mm, wherein the aerosol generating matrix comprises about 340 mg of homogenized rosemary material in the form of multiple thin strips, wherein the homogenized rosemary material comprises about 14% by weight of glycerol on a dry weight basis. In this embodiment, the aerosol generating article has a total length of about 74 mm and includes a cellulose acetate tow filter with a length of about 10 mm and an end cavity defined by a hollow tube with a length of about 6-7 mm. The aerosol generating article is contained in a hollow tube downstream of the aerosol generating matrix, wherein the hollow tube has a length of about 25 mm and is provided with a ventilation zone.
[0249] The aerosol-generating article according to the present invention may have a total length of at least about 30 mm or at least about 40 mm. The total length of the aerosol-generating article may be less than 90 mm or less than about 80 mm.
[0250] In one embodiment, the aerosol-generating article has an overall length of about 40 mm to about 50 mm, preferably about 45 mm. In another embodiment, the aerosol-generating article has an overall length of about 70 mm to about 90 mm, preferably about 80 mm to about 85 mm. In yet another embodiment, the aerosol-generating article has an overall length of about 72 mm to about 76 mm, preferably about 74 mm.
[0251] 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.
[0252] The aerosol generating article according to the invention may further comprise one or more aerosol modifying elements. The aerosol modifying elements may provide aerosol modifiers. As used herein, the term aerosol modifier is used to describe any agent that modifies one or more characteristics or properties of aerosols passing through a filter in use. Suitable aerosol modifiers include, but are not limited to, agents that impart flavor or aroma to aerosols passing through a filter in use or agents that remove flavor from aerosols passing through a filter in use.
[0253] Aerosol modifiers can be one or more of water or liquid flavorings. Water or moisture can, for example, alter the user's sensory experience by wetting the generated aerosol, providing a cooling effect to the aerosol and reducing the irritation experienced by the user. Aerosol modifiers can be in the form of flavoring delivery elements for delivering one or more liquid flavorings. Alternatively, liquid flavorings can be added directly to homogenized rosemary material, for example, by adding flavorings to the pulp or raw material during the production of homogenized rosemary material, or by spraying liquid flavorings onto the surface of homogenized rosemary material.
[0254] One or more liquid flavoring agents may comprise any flavoring compound or plant extract, said flavoring compound or plant extract being suitably disposed in liquid form within the flavoring delivery element to enhance the flavor of the aerosol generated during the use of the aerosol-generating article. Liquid or solid flavoring agents may also be disposed directly within a filter-forming material such as cellulose acetate tow. Suitable flavorings or flavorings include, but are not limited to, menthol, peppermint such as peppermint and spearmint, chocolate, licorice, citrus and other fruit flavorings, gamma-octanol, vanillin, ethyl vanillin, breath freshener flavorings, spices such as cinnamon, methyl salicylate, linalool, eugenol, bergamot oil, geranium oil, lemon oil, and tobacco flavorings. Other suitable flavorings may include flavor compounds selected from acids, alcohols, esters, aldehydes, ketones, pyrazines, combinations thereof, or blends thereof.
[0255] In some embodiments of the invention, the aerosol modifier may be an essential oil derived from one or more plants. For example, homogenized rosemary materials may contain rosemary oil, such as rosemary essential oil, to further enhance the rosemary flavor delivered to the consumer when heated.
[0256] In some embodiments of the invention, the aerosol generating matrix may comprise homogenized rosemary material, which, in combination with rosemary oil, comprises particulate plant material, such as tea particles.
[0257] Aerosol modifiers can be adsorbent materials such as activated carbon, which remove certain aerosol components that pass through a filter and thereby alter the flavor and aroma of the aerosol.
[0258] One or more aerosol-modifying elements may be located downstream of or within the aerosol-generating matrix. The aerosol-generating matrix may include homogenized rosemary material and the aerosol-modifying elements. In various embodiments, the aerosol-modifying elements may be placed adjacent to or embedded in the homogenized rosemary material. Typically, the aerosol-modifying elements may be located downstream of the aerosol-generating matrix, most commonly within an aerosol cooling element, within a filter of the aerosol-generating article, such as within a filter tip section or cavity, preferably within a cavity between filter tip sections. The one or more aerosol-modifying elements may be in the form of threads, capsules, microcapsules, beads, or polymer matrix materials, or combinations thereof.
[0259] If the aerosol modifier element is in the form of a line, as described in WO-A-2011 / 060961, the line can be formed from paper, such as filter tip segments, and the line can contain at least one aerosol modifier and be located within the filter body. Other materials that can be used to form the line include cellulose acetate and cotton.
[0260] If the aerosol conditioning element is in capsule form, as described in WO-A-2007 / 010407, WO-A-2013 / 068100, and WO-A-2014 / 154887, the capsule can be a breakable capsule located within the filter. The capsule's core contains an aerosol conditioner that can be released when the capsule shell breaks under external force on the filter. The capsule can be located within the filter tip section or cavity, preferably within the cavity between the filter tip sections.
[0261] If the aerosol modifying element is in the form of a polymer matrix, then when the aerosol-generating article is heated, for example, when the polymer matrix is heated above its melting point, the polymer matrix releases a flavoring agent, as described in WO-A-2013 / 034488. Typically, such a polymer matrix can be located within beads within the aerosol-generating matrix. Alternatively or additionally, the flavoring agent can be trapped within a domain of the polymer matrix and released from the polymer matrix upon compression. Preferably, the flavoring agent is released when the polymer matrix is compressed with a force of about 15 Newtons. Such a flavor modifying element can provide a sustained release of liquid flavoring agents with a force of at least 5 Newtons, in the range of 5N to 20N, as described in WO2013 / 068304. Typically, such a polymer matrix can be located within beads within a filter.
[0262] The aerosol generating article may include a combustible heat source and an aerosol generating matrix downstream of the combustible heat source, wherein the aerosol generating matrix is as described above with respect to the first aspect of the present invention.
[0263] For example, the matrix described herein can be used in heated aerosol generating articles of the type disclosed in WO-A-2009 / 022232, which include a combustible carbon-based heat source, an aerosol generating matrix downstream of the combustible heat source, and a thermally conductive element surrounding and contacting the rear portion of the combustible carbon-based heat source and the adjacent front portion of the aerosol generating matrix. However, it should be understood that the matrix described herein can also be used in heated aerosol generating articles comprising combustible heat sources having other configurations.
[0264] The present invention provides an aerosol generation system comprising an aerosol generation apparatus including a heating element, and an aerosol generation article used with the aerosol generation apparatus, the aerosol generation article comprising the aerosol generation matrix as described above.
[0265] In a preferred embodiment, the aerosol generating matrix as described herein can be used in a heated aerosol generating article used in an electrically operated aerosol generating system, wherein the aerosol generating matrix of the heated aerosol generating article is heated by an electric heating source.
[0266] For example, the aerosol generating matrix as described herein can be used in heated aerosol generating articles of the type disclosed in EP-A-0 822 760.
[0267] The heating element of such an aerosol generating device can be of any suitable form for heat conduction. Heating of the aerosol generating matrix can be achieved internally, externally, or both internally and externally. The heating element is preferably a heater blade or pin adapted to be inserted into the matrix so that the matrix is heated from the inside. Alternatively, the heating element can partially or completely surround the matrix and heat the matrix circumferentially from the outside.
[0268] The aerosol generation system can be an electrically operated aerosol generation system including an induction heating device. The induction heating device typically includes an induction source configured to couple with a sensor, which can be disposed outside or inside the aerosol generation matrix. The induction source generates an alternating electromagnetic field that induces magnetization or eddy currents in the sensor. The sensor can be heated due to hysteresis losses or induced eddy currents, which are achieved through ohmic or resistive heating.
[0269] An electrically operated aerosol generation system including an induction heating device may also include an aerosol generation article having an aerosol generation matrix and a sensor in thermal proximity to the aerosol generation matrix. Typically, the sensor is in direct contact with the aerosol generation matrix, and heat is transferred from the sensor to the aerosol generation matrix primarily through conduction. Examples of electrically operated aerosol generation systems with induction heating devices and aerosol generation articles with sensors are described in WO-A1-95 / 27411 and WO-A1-2015 / 177255.
[0270] The receptors can be multiple receptor particles, which can be deposited on or embedded within the aerosol-generating matrix. When the aerosol-generating matrix is in the form of one or more sheets, multiple receptor particles can be deposited on or embedded within the one or more sheets. The receptor particles are fixed by, for example, the matrix in sheet form and held in their initial positions. Preferably, the receptor particles can be uniformly distributed in a homogenized rosemary material of the aerosol-generating matrix. Due to the particulate nature of the receptors, heat is generated according to the distribution of the particles in the homogenized rosemary material sheet of the matrix. Alternatively, one or more sheets, strips, fragments, or strips of receptors can be placed next to or embedded in the homogenized rosemary material. In one embodiment, the aerosol-forming matrix contains one or more receptor strips. For example, a strip of the aerosol-generating matrix can contain elongated receptor elements extending longitudinally therethrough. In another embodiment, the receptors are present in an aerosol-generating apparatus.
[0271] The receptor may have a heat loss greater than 0.05 joules / kg, preferably greater than 0.1 joules / kg. Heat loss is the ability of the receptor to transfer heat to the surrounding material. Because the receptor particles are preferably uniformly distributed in the aerosol-generating matrix, uniform heat loss from the receptor particles can be achieved, thus generating a uniform heat distribution in the aerosol-generating matrix and resulting in a uniform temperature distribution in the aerosol-generating article. It has been found that a minimum heat loss of 0.05 joules / kg in the receptor particles allows the aerosol-generating matrix to be heated to a substantially uniform temperature, thereby providing aerosol generation. Preferably, in such embodiments, the average temperature achieved within the aerosol-generating matrix is from about 200 degrees Celsius to about 240 degrees Celsius.
[0272] The risk of overheating the aerosol generation matrix can be mitigated by using a sensor material with a Curie temperature, allowing the process to be heated only to a maximum temperature due to hysteresis losses. The sensor may have a Curie temperature between about 200°C and about 450°C, preferably between about 240°C and about 400°C, for example, about 280°C. When the sensor material reaches its Curie temperature, its magnetic properties change. At the Curie temperature, the sensor material changes from a ferromagnetic phase to a paramagnetic phase. Heating based on energy loss ceases due to the orientation of the ferromagnetic domains. Furthermore, heating is primarily based on eddy current formation, causing the heating process to automatically decrease upon reaching the Curie temperature of the sensor material. Preferably, the sensor material and its Curie temperature are adapted to the composition of the aerosol generation matrix to achieve optimal temperature and temperature distribution within the aerosol generation matrix for optimal aerosol generation.
[0273] In some preferred embodiments of the aerosol-generating article according to the invention, the receptor is made of ferrite. Ferrite is a ferromagnetic material with high magnetic permeability and is particularly suitable as a receptor material. The main component of ferrite is iron. Other metallic components, such as zinc, nickel, manganese, or non-metallic components such as silicon, may be present in varying amounts. Ferrite is a relatively inexpensive commercially available material. Ferrite can be obtained in particulate form, with a size range corresponding to the size range of particles used to form the homogenized rosemary material according to the invention. Preferably, the particles are fully sintered ferrite powders, such as FP160, FP215, and FP350 manufactured by PPT in Indiana, USA.
[0274] In some embodiments of the invention, the aerosol generation system includes an aerosol generation article comprising an aerosol generation matrix as defined above, an aerosol forming agent source, and means for evaporating the aerosol forming agent, preferably a heating element as described above. The aerosol forming agent source may be a refillable or replaceable reservoir located on the aerosol generation apparatus. When the reservoir is physically separated from the aerosol generation article, the generated vapor is directed through the aerosol generation article. The vapor contacts the aerosol generation matrix, which releases volatile compounds, such as nicotine and flavorings from particulate plant material, to form an aerosol. Optionally, to facilitate the volatilization of compounds in the aerosol generation matrix, the aerosol generation system may also include a heating element to heat the aerosol generation matrix, preferably in a manner coordinated with the aerosol forming agent. However, in some embodiments, the heating element for heating the aerosol generation article is separate from the heater for heating the aerosol forming agent.
[0275] As defined above, the present invention also provides an aerosol generated during the heating of an aerosol-generating matrix, wherein the aerosol comprises a specific amount and ratio of characteristic compounds derived from rosemary particles as defined above.
[0276] According to the present invention, the aerosol comprises: at least 0.5 micrograms of betulinic acid per aspiration; at least 0.01 micrograms of rosmarinic acid per aspiration; and at least 0.01 micrograms of 12-O-methylsarstilin per aspiration, wherein, if generated by a fumigation machine, a single aspiration of the aerosol has a volume of 55 ml. For the purposes of this invention, "aspiration" is defined as the volume of aerosol released from the aerosol-generating matrix upon heating and collected for analysis, wherein, if generated by a fumigation machine, the aspiration of the aerosol has a volume of 55 ml. Therefore, unless otherwise stated, any reference herein to "aspiration" of an aerosol should be understood to mean a 55 ml aspiration.
[0277] The indicated range defines the total amount of each component measured in a 55 ml aerosol aspiration. Aerosols can be generated from an aerosol-generating matrix using any suitable device and can be captured and analyzed as described above to identify characteristic compounds within the aerosol and measure their quantity. For example, “aspiration” can correspond to a 55 ml aspiration performed on a smoking machine, as used in the Health Canada test method described herein.
[0278] Preferably, the aerosol according to the invention comprises at least about 0.5 micrograms of betulinic acid per aerosol aspiration, more preferably at least about 2 micrograms of betulinic acid per aerosol aspiration, and even more preferably at least about 5 micrograms of betulinic acid per aerosol aspiration. Alternatively or additionally, the aerosol generated from the aerosol generating matrix comprises up to about 25 micrograms of betulinic acid per aerosol aspiration, preferably up to about 20 micrograms of betulinic acid per aerosol aspiration, and even more preferably up to about 15 micrograms of betulinic acid per aerosol aspiration. For example, the aerosol generated from the aerosol generating matrix may comprise about 0.5 micrograms to about 25 micrograms of betulinic acid per aerosol aspiration, or about 2 micrograms to about 20 micrograms of betulinic acid per aerosol aspiration, or about 5 micrograms to about 15 micrograms of betulinic acid per aerosol aspiration.
[0279] Preferably, the aerosol according to the invention comprises at least about 0.1 micrograms of rosmarinic acid per aerosol aspiration, more preferably at least about 0.5 micrograms of rosmarinic acid per aerosol aspiration. Alternatively or additionally, the aerosol generated from the aerosol generating matrix preferably comprises up to about 5 micrograms of rosmarinic acid per aerosol aspiration, more preferably up to about 2 micrograms of rosmarinic acid per aerosol aspiration, and even more preferably up to about 1 microgram of rosmarinic acid per aerosol aspiration. For example, the aerosol generated from the aerosol generating matrix may comprise about 0.01 micrograms to about 5 micrograms of rosmarinic acid per aerosol aspiration, or about 0.1 micrograms to about 2 micrograms of rosmarinic acid per aerosol aspiration, or 0.5 micrograms to 1 microgram of rosmarinic acid per aerosol aspiration.
[0280] Preferably, the aerosol according to the invention comprises at least about 0.1 micrograms of 12-O-methylcaryophyllin per aerosol aspiration, more preferably at least about 0.5 micrograms of 12-O-methylcaryophyllin per aerosol aspiration. Alternatively or additionally, the aerosol generated from the aerosol generating matrix preferably comprises up to about 5 micrograms of 12-O-methylcaryophyllin per aerosol aspiration, more preferably up to about 2 micrograms of 12-O-methylcaryophyllin per aerosol aspiration, and even more preferably up to about 1 microgram of 12-O-methylcaryophyllin per aerosol aspiration. For example, the aerosol generated by the aerosol generating matrix may contain about 0.01 micrograms to about 5 micrograms of 12-O-methylcaryophyllin in each aerosol extraction, or about 0.1 micrograms to about 2 micrograms of 12-O-methylcaryophyllin in each aerosol extraction, or about 0.5 micrograms to about 1 microgram of 12-O-methylcaryophyllin in each aerosol extraction.
[0281] According to the present invention, the aerosol composition is such that the amount of betulinic acid in each aerosol aspiration is preferably at least about 5 times the amount of rosmarinic acid in each aerosol aspiration. Therefore, the ratio of betulinic acid to rosmarinic acid in the aerosol is preferably at least about 5:1.
[0282] Preferably, the amount of betulinic acid in each aerosol aspiration is at least 10 times the amount of rosmarinic acid in each aerosol aspiration. More preferably, the amount of betulinic acid in each aerosol aspiration is at least 20 times the amount of rosmarinic acid in each aerosol aspiration.
[0283] The defined ratio of betulinic acid to rosmarinic acid characterizes aerosols derived from rosemary particles. In contrast, the ratio of betulinic acid to rosmarinic acid would be significantly different in aerosols produced from rosemary essential oil.
[0284] Preferably, the aerosol according to the invention further comprises at least about 0.1 mg of aerosol forming agent per aspiration, more preferably at least about 0.2 mg of aerosol per aspiration, and even more preferably at least about 0.3 mg of aerosol forming agent per aspiration. Preferably, the aerosol comprises up to 0.6 mg of aerosol forming agent per aspiration, more preferably up to 0.5 mg of aerosol forming agent per aspiration, and even more preferably up to 0.4 mg of aerosol forming agent per aspiration. For example, the aerosol may comprise about 0.1 mg to about 0.6 mg of aerosol forming agent per aspiration, or about 0.2 mg to about 0.5 mg of aerosol forming agent per aspiration, or about 0.3 mg to about 0.4 mg of aerosol forming agent per aspiration. These values are based on a 55 mL aspiration volume as defined above.
[0285] Suitable aerosol forming agents for use in this invention are as described above.
[0286] Preferably, the aerosol generated from the aerosol generating matrix according to the invention further comprises at least about 2 micrograms of nicotine per aspirated aerosol, more preferably at least about 20 micrograms of nicotine per aspirated aerosol, and even more preferably at least about 40 micrograms of nicotine per aspirated aerosol. Preferably, the aerosol comprises up to about 200 micrograms of nicotine per aspirated aerosol, more preferably up to about 150 micrograms of nicotine per aspirated aerosol, and even more preferably up to about 75 micrograms of nicotine per aspirated aerosol. For example, the aerosol may comprise about 2 to about 200 micrograms of nicotine per aspirated aerosol, or about 20 to about 150 micrograms of nicotine per aspirated aerosol, or about 40 to about 75 micrograms of nicotine per aspirated aerosol. These values are based on a 55 ml aspirated volume as defined above. In some embodiments of the invention, the aerosol may contain zero micrograms of nicotine.
[0287] Carbon monoxide may also be present in the aerosols according to the invention and can be measured and used for further characterization of the aerosols. Nitrogen oxides, such as nitric oxide and nitrogen dioxide, may also be present in the aerosols and can be measured and used for further characterization of the aerosols.
[0288] Aerosols according to the invention, containing characteristic compounds from rosemary particles, can be formed from particles with a mass median aerodynamic diameter (MMAD) ranging from about 0.01 to 200 micrometers or from about 1 to 100 micrometers. Preferably, when the aerosol contains nicotine as described above, the aerosol contains particles having an MMAD ranging from about 0.1 to about 3 micrometers to optimize the delivery of nicotine from the aerosol.
[0289] The mass median aerodynamic diameter (MMAD) of an aerosol refers to the aerodynamic diameter at which half the particle mass is contributed by particles with an aerodynamic diameter greater than MMAD and the other half by particles with an aerodynamic diameter less than MMAD. The aerodynamic diameter is defined as the diameter of particles with a density of 1 g / cm³. 3 The diameter of the spherical particle, which has the same settling velocity as the characterized particle.
[0290] 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.
[0291] As defined above, the present invention also provides an aerosol generating article comprising an aerosol generating matrix, the aerosol generating matrix comprising homogenized rosemary material, wherein when the aerosol generating matrix is heated according to test method A, the aerosol generated from the aerosol generating matrix comprises: at least 0.5 micrograms of betulinic acid per aspirated aerosol; at least 0.01 micrograms of rosmarinicotinic acid per aspirated aerosol; and at least 0.01 micrograms of 12-O-methylsalazine per aspirated aerosol, wherein, if generated by a smoking machine, a single aspirated aerosol has a volume of 55 ml.
[0292] For the purposes of this invention, “aspiration” is defined as the volume of aerosol released from the aerosol-generating matrix upon heating and collected for analysis, wherein, if generated by a smoking machine, the aspiration of the aerosol has a 55 mL aspiration volume. Therefore, unless otherwise stated, any reference herein to “aspiration” of aerosol should be understood to mean a 55 mL aspiration. The indicated range defines the total amount of each component measured in a 55 mL aspiration of aerosol. Aerosols can be generated from the aerosol-generating matrix 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, “aspiration” may correspond to a 55 mL aspiration performed on a smoking machine, as used in the Health Canada test method described herein.
[0293] Preferably, the amount of betulinic acid in each aerosol aspiration is at least 5 times the amount of rosmarinic acid in each aerosol aspiration, more preferably at least 10 times the amount of rosmarinic acid in each aerosol aspiration, and even more preferably at least 20 times the amount of rosmarinic acid in each aerosol aspiration.
[0294] As defined above, the present invention also provides an aerosol-generating matrix formed from homogenized rosemary material, said homogenized rosemary material comprising 1% to 25% by weight of rosemary particles, about 5% to 30% by weight of an aerosol forming agent and 1% to 10% by weight of a binder, wherein said aerosol-generating matrix comprises: at least 30 micrograms of betulinic acid per gram matrix on a dry weight basis; at least 1 microgram of rosmarinicotinic acid per gram matrix on a dry weight basis; and at least 1 microgram of 12-O-methylsalazine per gram matrix on a dry weight basis.
[0295] Specific implementation schemes will be further described by way of example only with reference to the accompanying drawings, in which:
[0296] Figure 1 A first embodiment of a matrix for an aerosol-generated article as described herein is shown;
[0297] Figure 2 An aerosol generation system is shown, comprising an aerosol generating article and an aerosol generating apparatus, the aerosol generating apparatus including an electric heating element;
[0298] Figure 3 An aerosol generation system is shown, comprising an aerosol generating article and an aerosol generating apparatus, the aerosol generating apparatus including a combustible heating element;
[0299] Figure 4a and 4b A second embodiment of the matrix for the aerosol-generated article as described herein is shown;
[0300] Figure 5 A third embodiment of the matrix for the aerosol-generated article as described herein is shown;
[0301] Figures 6a-6c This is a cross-sectional view of a filter 1050 that also includes an aerosol modification element, wherein...
[0302] Figure 6a The aerosol modification element in the form of spherical capsules or beads is shown within the filter tip section.
[0303] Figure 6b The aerosol modification element in the form of a line is shown in the filter tip section.
[0304] Figure 6c The aerosol modification element, in the form of a spherical capsule, is shown inside the cavity of the filter;
[0305] Figure 7 A cross-sectional view of a rod comprising an aerosol-generating matrix 1020, which also includes elongated sensory elements; and
[0306] Figure 8 The diagram illustrates an experimental setup for collecting aerosol samples to be analyzed in order to measure characteristic compounds.
[0307] Figure 1 A heated aerosol-generating article 1000 comprising a matrix as described herein is illustrated. Article 1000 comprises four elements: an aerosol-generating matrix 1020, a hollow cellulose acetate tube 1030, a spacer element 1040, and a mouthpiece filter 1050. These four elements are arranged sequentially and coaxially aligned, and assembled from cigarette paper 1060 to form the aerosol-generating article 1000. Article 1000 has a mouth end 1012 inserted into his or her mouth during use, and a distal end 1013 located at the end of the article opposite the mouth end 1012. Figure 1 The embodiment of the aerosol-generating article illustrated in the figure is particularly suitable for use with an electrically operated aerosol-generating apparatus that includes a heater for heating the aerosol-generating matrix.
[0308] During assembly, article 1000 has a length of approximately 45 mm and an outer diameter of approximately 7.2 mm and an inner diameter of approximately 6.9 mm.
[0309] The aerosol generating matrix 1020 comprises a rod formed from a sheet of homogenized rosemary material, the homogenized rosemary material comprising individual rosemary particles or a combination of rosemary particles and tobacco particles.
[0310] Table 1 below shows several examples of suitable homogenized plant materials for forming aerosol-generating matrix 1020 (see samples B through D). Sheets are aggregated, pressed, and wrapped in filter paper (not shown) to form rods. The sheets contain additives, including glycerol as an aerosol forming agent.
[0311] like Figure 1 The aerosol generating article 1000 shown is designed to be coupled to an aerosol generating apparatus for consumption. Such an aerosol generating apparatus includes means for heating the aerosol generating matrix 1020 to a sufficient temperature to form an aerosol. Typically, the aerosol generating apparatus may include a heating element adjacent to the aerosol generating matrix 1020 surrounding the aerosol generating article 1000, or a heating element inserted into the aerosol generating matrix 1020.
[0312] Once connected to the aerosol generating device, the user inhales through the mouthpiece 1012 of the smoking article 1000, and the aerosol generating matrix 1020 is heated to a temperature of approximately 375 degrees Celsius. At this temperature, volatile compounds are released from the aerosol generating matrix 1020. These compounds condense to form an aerosol. The aerosol is then drawn through the filter 1050 and into the user's mouth.
[0313] Figure 2 A portion of an electrically operated aerosol generation system 2000 is shown, which utilizes heating blades 2100 to heat the aerosol generation matrix 1020 of an aerosol generation article 1000. The heating blades are mounted within the aerosol article receiving chamber of the electrically operated aerosol generation apparatus 2010. The aerosol generation apparatus defines a plurality of air holes 2050 to allow airflow to the aerosol generation article 1000. The airflow is... Figure 2 The arrow above indicates this. The aerosol generating device includes a power supply and electronic components, which are not located in... Figure 2 As shown in the image. Figure 2 The aerosol-generated products 1000 are as follows: Figure 1 As described.
[0314] exist Figure 3 In the alternative configuration shown, the aerosol generation system is depicted as having a combustible heating element. Although Figure 1 Product 1000 is intended for use in conjunction with an aerosol generating device, but Figure 3 Article 1001 includes a combustible heat source 1080, which can be ignited and transfer heat to an aerosol-generating matrix 1020 to form an inhalable aerosol. The combustible heat source 80 is a charcoal element assembled at the distal end 13 of strip 11 close to the aerosol-generating matrix. Figure 1 Components that are essentially the same are assigned the same number.
[0315] Figure 4a and 4b Second embodiments 4000a and 4000b of the heated aerosol-generating article are illustrated. The aerosol-generating matrices 4020a and 4020b include a first downstream rod 4021 formed of granular plant material containing rosemary particles and a second upstream rod 4022 formed of granular plant material primarily containing tobacco particles. Suitable homogenizing plant material used in the first downstream rod is shown in Table 1 below as one of samples B to D. Suitable homogenizing plant material used in the second upstream rod is shown in Table 1 below as sample A. Sample A contains only tobacco particles and is included only for comparative purposes.
[0316] In each rod, homogenized plant material is in sheet form, which is pressed and wrapped in filter paper (not shown). Both sheets contain additives, including glycerol as an aerosol forming agent. Figure 4a In the illustrated embodiment, the sticks are joined end-to-end in an adjacent relationship to form a strip, and each stick has an equal length of approximately 6 mm. In a more preferred embodiment (not shown), the second stick is preferably longer than the first stick, for example, preferably 2 mm longer, more preferably 3 mm longer, such that the length of the second stick is 7 or 7.5 mm while the length of the first stick is 5 or 4.5 mm, to provide a desired tobacco to rosemary particle ratio in the matrix. Figure 4b The cellulose acetate tube support element 1030 is omitted in the original text.
[0317] Similar to Figure 1 Products 1000, 4000a, and 4000b are particularly suitable for use with, including Figure 2 The heater shown is used in conjunction with the electrically operated aerosol generation system 2000. Figure 1 Components that are essentially the same are assigned the same numbering. Those skilled in the art can conceive of this in relation to... Figure 3 In a similar configuration to the configuration of the article 1001 containing a combustible heat source 1080, the combustible heat source (not shown) may alternatively replace the electric heating element and be used with the second embodiment.
[0318] Figure 5 A third embodiment 5000 of a heated aerosol-generating article is illustrated. The aerosol-generating matrix 5020 includes a strip formed from a first homogenized rosemary material sheet and a second homogenized plant material sheet. The first homogenized rosemary material sheet is formed from granular plant material containing a certain proportion of rosemary particles, and the second homogenized plant material sheet mainly contains cast tobacco leaves.
[0319] Suitable homogenized rosemary material for use as the first sheet is shown in Table 1 below as one of samples B to D. Suitable homogenized plant material for use as the second sheet is shown in Table 1 below as sample A. Sample A contains only tobacco particles and is included only for comparative purposes.
[0320] A second sheet is overlaid on the first sheet, and the combined sheets have been pressed, aggregated, and at least partially wrapped in filter paper (not shown) to form a rod as part of a strip. Both sheets contain additives, including glycerol as an aerosol forming agent. Similar to Figure 1 Products 1000 and 5000 are particularly suitable for products including Figure 2 The heater shown is used in conjunction with the electrically operated aerosol generation system 2000. Figure 1 Components that are essentially the same are assigned the same numbering. Those skilled in the art can conceive of this in relation to... Figure 3In a similar configuration to the configuration of the article 1001 containing a combustible heat source 1080, the combustible heat source (not shown) may alternatively replace the electric heating element and be used with the third embodiment.
[0321] Figures 6a-6c This is a cross-sectional view of a filter 1050 that also includes an aerosol modification element. Figure 6a In the filter 1050, there is also an aerosol modification element in the form of spherical capsules or beads 605.
[0322] exist Figure 6a In one embodiment, the capsule or bead 605 is embedded in the filter section 601 and surrounded on all sides by filter material 603. In this embodiment, the capsule comprises a shell and a core, and the core contains a liquid flavoring agent. The liquid flavoring agent is used to flavor the aerosol during use of the aerosol-generating article provided with the filter. When the filter is subjected to external force, such as when squeezed by a consumer, the capsule 605 releases at least a portion of the liquid flavoring agent. In the illustrated embodiment, the capsule is generally spherical and has a substantially continuous shell containing the liquid flavoring agent.
[0323] exist Figure 6b In one embodiment, the filter section 601 includes a rod of filter material 603 and a central flavor-carrying line 607 extending through the rod of filter material 603, parallel to the longitudinal axis of the filter 1050. The length of the central flavor-carrying line 607 is substantially the same as the length of the filter material rod 603, such that the end of the central flavor-carrying line 607 is visible at the end of the filter section 601. Figure 6b In this process, the filter material 603 is a cellulose acetate tow. The central flavor carrier line 607 is formed by packaging twisted filter tip segments and is loaded with an aerosol modifier.
[0324] exist Figure 6c In one embodiment, filter segment 601 includes more than one filter material rod 603, 603'. Preferably, filter material rods 603, 603' are formed of cellulose acetate, enabling them to filter aerosols provided by the aerosol-generating article. Package 609 encloses and connects the filter tip segments 603, 603'. Within cavity 611 is a capsule 605 comprising a shell and a core, the core containing a liquid flavoring agent. This capsule is otherwise similar to Figure 6a The implementation plan.
[0325] Figure 7This is a cross-sectional view of an aerosol generating matrix 1020, which also includes elongated receptor strips 705. The aerosol generating matrix 1020 comprises a rod 703 formed from a sheet of homogenized rosemary material containing tobacco particles and rosemary particles. The elongated receptor strips 705 are embedded within the rod 703 and extend longitudinally between the upstream and downstream ends of the rod 703. During use, the elongated receptor strips 705 heat the homogenized rosemary material by means of induction heating as described above.
[0326] Example
[0327] As described above with reference to the accompanying drawings, different samples of homogenized plant materials for use as aerosol-generating matrices according to the present invention can be prepared from aqueous slurries having the compositions shown in Table 1. Samples B to D according to the present invention contain rosemary particles and tobacco particles. Sample A contains only tobacco particles and is included only for comparative purposes.
[0328] In all samples A through D, granular plant material comprised 75% of the dry weight of the homogenized plant material, while glycerol, guar gum, and cellulose fibers comprised the remaining 25%. The samples were prepared from an aqueous pulp containing 78-79 kg of water per 100 kg of pulp.
[0329] In the table below, % DWB refers to "dry weight basis," in which case the weight percentage is calculated relative to the dry weight of the homogenized plant material. Rosemary powder is available from Spain. rosemary Leaf formation can be achieved by grinding the leaf into a final D95 = 133 micrometers through triple impact milling.
[0330] The paste 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.
[0331] Table 1. Dry content of slurry
[0332]
[0333] For each of samples A through D of the homogenized plant material, a rod is produced from a single continuous sheet of the homogenized plant material, each sheet having a width of 100 mm to 125 mm. Each sheet preferably has a thickness of approximately 220 micrometers and a g / m³ of approximately 200 g / m². 2 The weight per square meter. The cutting width of each sheet can be adjusted based on the thickness of each sheet to produce strips of comparable volume. The sheets are pressed to a height of 165 to 170 micrometers and rolled into rods with a length of approximately 12 mm and a diameter of approximately 7 mm, and then wrapped with wrapping paper.
[0334] For each rod, an aerosol-generating article with a total length of approximately 45 mm can be formed, which has the following properties: Figure 3 The structure shown includes, from the downstream end: an inlet-side cellulose acetate filter (approximately 7 mm long), an aerosol spacer comprising a press-fit sheet of polylactic acid polymer (approximately 18 mm long), a hollow cellulose acetate tube (approximately 8 mm long), and a rod of aerosol generating matrix.
[0335] For samples of homogenized rosemary material containing rosemary particles, characteristic rosemary compounds can be extracted from the rods of homogenized rosemary material using methanol, as detailed above. The extract can be analyzed as described above to confirm the presence of characteristic compounds and to measure their amounts. This can be used to confirm that the levels of characteristic compounds are within the defined ranges set forth above. Therefore, the analysis can be used to provide quality control of the aerosol-generating matrix. For example, the extract can be analyzed to confirm that the levels of betulinic acid, rosmarinic acid, and 12-O-methylsalpinx are within the ranges listed in Table 2 below.
[0336] Table 2. Amount of rosemary-specific compounds in the aerosol-forming matrix
[0337]
[0338] Mainstream aerosols of aerosol-generating products, which incorporate aerosol-generating matrices formed from homogenized plant materials (samples A to D), can be generated according to test method A as defined above. For each sample, the generated aerosols can be captured and analyzed.
[0339] As described in detail above, according to Test Method A, the commercially available iQOS® Heated Tobacco System 2.2 Holder (THS2.2 Holder) (from Philip Morris Products SA) can be used to test aerosol-generating articles. The aerosol-generating article is heated according to the Health Canada machine smoking protocol for more than 30 puffs, 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).
[0340] Aerosols generated during the smoking test were collected on a Cambridge filter pad and extracted with a liquid solvent. Figure 8 Suitable apparatus for generating and collecting aerosols from aerosol-generated articles is shown.
[0341] Figure 8The 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 the aerosol collection line 120. The glass fiber filter pad 140 is a 44mm Cambridge glass fiber filter pad (CFP) according to ISO 4387 and ISO 3308.
[0342] For LC-HRAM-MS analysis :
[0343] Extraction solvents 170 and 170a are, in this case, methanol and internal standard (ISTD) solutions, each with a volume of 10 mL in each micro dust detector 160 and 160a. Cold baths 161 and 161a each contain dry ice-isopropyl ether to maintain micro dust detectors 160 and 160a at approximately -60°C, whereby the gas-vapor phase is captured in extraction solvents 170 and 170a as aerosol bubbles pass through them. In step 181, the combined solution from the two micro dust detectors is separated into a gas-vapor phase solution 180 captured by the dust detectors.
[0344] In step 190, the CFP and the gas-vapor phase solution 180 captured by the dust detector are combined in a clean Pyrex® tube. In step 200, total particulate matter is extracted from the CFP using the gas-vapor phase solution 180 (containing methanol as a solvent) by thorough shaking (to disintegrate the CFP), vortexing for 5 minutes, and finally centrifugation (4500 g, 5 min, 10 °C). An aliquot (300 μL) of the reconstituted total aerosol extract 220 is transferred to a silanized chromatographic vial and diluted with methanol (700 μL), as 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).
[0345] Aliquots (1.5 μL) of diluted extract were injected and analyzed by LC-HRAM-MS in full scan mode and data-dependent fracture mode for compound identification.
[0346] For GCxGC-TOFMS analysis:
[0347] As described above, different solvents are suitable for extracting and analyzing polar, nonpolar, and volatile compounds separated from the total aerosol when preparing GCxGC-TOFMS experimental samples. The experimental setup is the same as described for sample collection for LC-HRAM-MS, except as indicated below.
[0348] Nonpolar and polar
[0349] Extraction solvents 171 and 171a, present in 10 mL volumes, are 80:20 v / v mixtures of dichloromethane and methanol, and also contain retention index labeled (RIM) compounds and stable isotopically labeled internal standards (ISTDs). Cold baths 162 and 162a each contain a dry ice-isopropanol mixture to maintain micro dust detectors 160 and 160a at approximately -78°C. As aerosol bubbles pass through micro dust detectors 160 and 160a, the gas-vapor phase is captured in extraction solvents 171 and 171a. In step 182, the combined solution from the two micro dust detectors is separated into a gas-vapor phase solution 210 captured by the dust detectors.
[0350] nonpolar
[0351] In step 190, the CFP and the gas-vapor phase solution 210 captured by the dust detector are combined in a clean Pyrex® tube. In step 200, the total particulate matter from the CFP is extracted using the gas-vapor phase solution 210 captured by the dust detector (containing dichloromethane and methanol as solvents) by thorough shaking (to disintegrate the CFP), vortexing for 5 minutes, and finally centrifugation (4500 g, 5 min, 10 °C) to separate the polar and non-polar components of the total aerosol extract 230.
[0352] In step 250, a 10 mL aliquot of the total aerosol extract 230 is taken as sample 240. In step 260, 10 mL of water is added to the aliquot, and the entire sample is shaken and centrifuged. The nonpolar fraction 270 is separated, dried with sodium sulfate, and analyzed by GCxGC-TOFMS in full scan mode.
[0353] polarity
[0354] ISTD and RIM compounds were added to polar fraction 280 and then directly analyzed by GCxGC-TOFMS in full scan mode.
[0355] Each parallel smoking assay (n = 3) includes the cumulative capture and reconstructed nonpolar fraction 270 and polar fraction 280 for each sample.
[0356] Volatile components
[0357] The entire aerosol was captured using two tandem micro-dust collectors 160 and 160a. Extraction solvents 172 and 172a in this case were N,N-dimethylformamide (DMF) containing a retention index-labeled (RIM) compound and a stable isotopically labeled internal standard (ISTD), with a volume of 10 mL in each micro-dust collector 160 and 160a. Cold baths 161 and 161a each contained dry ice-isopropyl ether to maintain micro-dust collectors 160 and 160a at approximately -60°C, and the gas-vapor phase was captured in extraction solvents 170 and 170a as the aerosol bubbled through the micro-dust collectors. In step 183, the combined solution from the two micro-dust collectors was separated into a volatile-containing phase 211. The volatile-containing phase 211 was analyzed separately from the other phases and injected directly into a GCxGC-TOFMS using on-column cooled injection without further preparation.
[0358] Table 3 below shows the levels of characteristic compounds from rosemary particles in aerosols generated from aerosol-generating articles according to the present invention, the aerosol-generating articles comprising an aerosol-generating matrix formed from homogenized rosemary material containing rosemary particles.
[0359] Table 3. Content of Rosemary Characteristic Compounds in Aerosols
[0360]
[0361] For example, relatively high levels of characteristic compounds will be measured in the aerosol generated from sample B. The ratio of betulinic acid to rosmarinic acid will typically be greater than 20:1. The level of characteristic compounds will therefore indicate the presence of rosemary particles in the sample. In contrast, for tobacco-only sample A, which contains virtually no rosemary particles, the level of characteristic compounds is found to be zero or close to zero.
Claims
1. An aerosol generating article comprising an aerosol generating matrix formed from homogenized rosemary material, the homogenized rosemary material comprising, by weight, 1% to 25% rosemary particles, 5% to 30% aerosol forming agent, and 1% to 10% a binder. The aerosol generating matrix comprises: At least 50 micrograms of betulinic acid per gram of the matrix, on a dry weight basis; At least 20 micrograms of rosmarinic acid per gram of the matrix, on a dry weight basis; and At least 0.3 micrograms of 12-O-methylsarstilin per gram of the matrix, on a dry weight basis.
2. The aerosol-generating article according to claim 1, wherein the amount of betulinic acid per gram of the matrix is at least 5 times the amount of rosmarinic acid per gram of the matrix.
3. The aerosol-generating article according to claim 1, wherein the aerosol-generating matrix comprises more than 0.5% by weight of 1,8-cineole.
4. The aerosol-generating article according to claim 1, wherein when the aerosol-generating matrix is heated according to test method A described in ISO / TR 19478-1:2014, the generated aerosol comprises: At least 30 micrograms of betulinic acid per gram of the matrix, on a dry weight basis; At least 1 microgram of rosmarinic acid per gram of the matrix, on a dry weight basis; and At least 1 microgram of 12-O-methylsarstilin per gram of the matrix, on a dry weight basis.
5. The aerosol-generating article according to claim 4, wherein the amount of betulinic acid per gram of the matrix is at least 5 times the amount of rosmarinic acid per gram of the matrix.
6. The aerosol-generated article according to any one of the preceding claims, wherein the homogenized rosemary material further comprises at least 40% by weight of tobacco particles on a dry weight basis.
7. The aerosol-generating article according to claim 6, wherein the homogenized rosemary material comprises 5% to 20% by weight of rosemary particles and 55% to 70% by weight of tobacco particles on a dry weight basis.
8. The aerosol-generating article of claim 1, wherein the aerosol-generating matrix comprises one or more sheets of the homogenized rosemary material, wherein each of the one or more sheets of the homogenized rosemary material individually comprises one or more of the following: Thickness from 100μm to 600μm; or 100g / m 2 Up to 300g / m 2 The weight per square meter.
9. The aerosol-generating article according to claim 1, wherein the homogenized rosemary material is in the form of a cast leaf.
10. The aerosol-generating article according to claim 1, wherein when the aerosol-generating matrix is heated according to test method A described in ISO / TR 19478-1:2014, the aerosol generated from the aerosol-generating matrix comprises: Each aerosol aspiration should contain at least 0.5 micrograms of betulinic acid; Each aspirate should contain at least 0.01 micrograms of rosmarinic acid; and Each aerosol aspiration should contain at least 0.01 micrograms of 12-O-methylcaryophyllin. The aerosol generated by the smoking machine has a volume of 55 ml per aspiration.
11. An aerosol-generating matrix formed from homogenized rosemary material, said homogenized rosemary material comprising 1% to 25% by weight of rosemary particles, 5% to 30% by weight of an aerosol forming agent, and 1% to 10% by weight of a binder. The aerosol generating matrix comprises: At least 30 micrograms of betulinic acid per gram of the matrix, on a dry weight basis; At least 1 microgram of rosmarinic acid per gram of the matrix, on a dry weight basis; and At least 1 microgram of 12-O-methylsarstilin per gram of the matrix, on a dry weight basis.
12. An aerosol generation system, the aerosol generation system comprising: Aerosol generating device including heating element; and The aerosol-generating product according to claim 1.
Citation Information
Patent Citations
Cigarette and heater for use in an electrical smoking system
EP0822760A2
Improvements relating to the production of tobacco smoking materials
GB983928A
Method of producing a reconstituted tobacco product
US3860012A
Process for producing tobacco structures
US3894544A
Reconstituted tobacco sheets and methods for producing and using the same
US5724998A