Dry shaped pellets, methods for their manufacture and uses thereof

Abstract

The present invention relates to shaped particles comprising a dry liquid composition comprising a plant extract, such as a tobacco extract. The invention also relates to a method for producing these dried shaped pellets and to the use thereof.

Description

TECHNICAL FIELD

[0001] The present invention relates to shaped particles comprising a dried liquid composition comprising a botanical extract, such as a tobacco extract. The invention also relates to methods of manufacturing these dried shaped particles and their use. BACKGROUND

[0002] It is a challenge to prepare a dried solid material from a liquid composition comprising a tobacco extract while retaining the desired components, including volatile or semi-volatile components. Dried material formed by conventional freeze-drying or lyophilisation methods typically forms a solid cake which is then broken up into particles of the desired size. SUMMARY

[0003] According to a first aspect of the invention, there is provided a shaped particle, each shaped particle comprising a freeze-dried shaped portion of a liquid composition, the liquid composition containing a botanical extract.

[0004] In some embodiments, the shaped particle comprises volatile and semi-volatile components of the botanical extract.

[0005] In some embodiments, the botanical extract is a tobacco extract and optionally an aqueous tobacco extract.

[0006] In some embodiments, the liquid composition further contains an aerosol-former material. In some embodiments, the aerosol-former material is glycerol.

[0007] In some embodiments, the liquid composition further contains an excipient. In some embodiments, the excipient is dextran.

[0008] In some embodiments, the shaped particle comprises about 45 to about 100% by weight of dried botanical extract (on a dry weight basis).

[0009] In some embodiments, the shaped particle comprises about 1 to about 20% by weight of aerosol-former material (on a dry weight basis).

[0010] In some embodiments, the shaped particle comprises about 0.1 to about 20% by weight of excipient (on a dry weight basis).

[0011] In some embodiments, the shaped particle is a freeze-dried droplet of the liquid composition containing the botanical extract.

[0012] In some embodiments, the shaped particle is a spheroid bead.

[0013] In some embodiments, at least 90% of the beads have a diameter that differs from the mass median diameter of the population by no more than 5%.

[0014] In some embodiments, the beads have a diameter in the range of about 2 mm to about 5 mm.

[0015] In some embodiments, the beads have a volume of about 0.005 to about 0.02 cm 3 .

[0016] In some embodiments, the shaped particles have a density in the range of about 0.5 to about 1.5 g / cm 3 .

[0017] In some embodiments, the shaped particles are flat in shape, such as a thin strip or disc.

[0018] In some embodiments, the shaped particles have a thickness of about 0.05 mm to about 1 mm.

[0019] In some embodiments, the shaped particles have a residual moisture content of no more than about 12% or no more than about 10%, as measured by Karl Fischer analysis.

[0020] In some embodiments, the residual moisture content is at least 7%, as measured by Karl Fischer analysis.

[0021] According to a second aspect of the application, there is provided a method of providing shaped particles, the method comprising: providing a portion of a liquid composition containing a plant extract in a mould; and freeze-drying the liquid composition in the mould.

[0022] In some embodiments, the method comprises: pre-freezing a droplet of the liquid composition containing a plant extract; and freeze-drying the frozen droplet to form a bead.

[0023] In some embodiments, the droplet of the liquid composition containing a plant extract has a volume of about 1 μΐ to about 50 μΐ.

[0024] In some embodiments, the droplet is pre-frozen by dispensing the droplet of the liquid composition into liquid nitrogen.

[0025] In some embodiments, the droplet is pre-frozen at atmospheric pressure.

[0026] In some embodiments, the droplet is instantaneously frozen on contact with the liquid nitrogen.

[0027] In some embodiments, the freeze-drying is performed at a temperature of about -35 to about -50°C.

[0028] In some embodiments, freeze drying is performed at a pressure of about 30 to about 40 μbar.

[0029] In some implementations, freeze-drying is carried out over a period of approximately 48 hours to approximately 120 hours.

[0030] In some implementations, the method includes a secondary drying step.

[0031] In some embodiments, the secondary drying step includes (involving) raising the temperature of the freeze-dried shaped particles to a secondary drying temperature not exceeding 20°C.

[0032] In some embodiments, the freeze-dried shaped granules are held at a secondary drying temperature for a period of about 9 hours to about 24 hours.

[0033] In some implementations, the secondary drying step is carried out at a pressure of about 20 to about 30 μbar.

[0034] According to a third aspect of the invention, a non-flammable sol supply system comprising molded particles according to the first aspect is provided.

[0035] In some implementations, the system is configured to heat-form particles to create vapor and / or aerosol.

[0036] In some embodiments, the non-flammable aerosol supply system includes other aerosol-generating materials that are heated to form aerosols and / or vapors. In some embodiments, the other aerosol-generating materials are liquids.

[0037] According to a fourth aspect of the invention, an article for use in a non-flammable aerosol supply system is provided, comprising molded granules according to the first aspect.

[0038] According to a fifth aspect of the invention, an oral product is provided, comprising a permeable container surrounding shaped particles according to the first aspect.

[0039] According to a sixth aspect, a method for providing an article of the fourth aspect or an oral product according to a fifth aspect is provided, the method comprising: One or more shaped particles are formed according to the method of the second aspect; and Place one or more shaped particles in a container.

[0040] According to the seventh aspect, the use of the molded particles according to any one of claims 1 to 20 for generating an inhalable medium is provided.

[0041] According to the eighth aspect, molded particles obtained or available by the method according to the second aspect are provided for use in an aerosol supply system to generate an inhalable medium. Attached Figure Description

[0042] Embodiments of the invention will now be described by way of example only with reference to the accompanying drawings, wherein: Figure 1 This is a side cross-sectional view of a first embodiment of a consumable comprising an aerosol generating material, the aerosol generating material comprising dried molded particles according to the invention.

[0043] Figure 2 It is used from Figure 1 A perspective view of a non-flammable aerosol supply device for generating aerosols from consumable aerosol generating materials.

[0044] Figure 3 This is a schematic diagram of a permeable container or bag for containing a group of dried, molded particles according to the present invention. Detailed Implementation

[0045] This invention relates to a plurality of molded particles (such as beads) or groups of molded particles, each molded particle comprising a dried or dehydrated molding portion of a liquid composition containing a plant extract. For example, the plant extract may be a tobacco extract.

[0046] As used herein, the term "shaped" refers to particles having a controlled and predetermined shape. For example, these particles are not formed by producing large dried clumps and then breaking them down into smaller particles. Such a process cannot provide particles with a controlled and predetermined shape. Instead, the liquid composition is dried in a pre-formed shape to form shaped particles. Different methods exist to achieve this, as discussed below.

[0047] Because each molded particle contains a dried molding portion of the liquid composition, multiple molded particles or groups of such molded particles have many advantageous properties. First, the composition of each molded particle can be precisely controlled. Second, the size and shape or form of each particle can be precisely controlled. Third, in some embodiments, the molded particles are free-flowing and easy to handle, store, and process.

[0048] Significantly, the ability to manufacture molded granules with predictable composition, size, and shape means that the granules can be used to provide accurate and predictable component delivery when in use. Furthermore, granule groups comprising mixtures of different granules (i.e., mixtures of granules with different properties) can be used to provide the desired delivery profile over a period of time.

[0049] Molded particles according to the invention can be prepared by freeze-drying a portion of the liquid composition in the desired shape.

[0050] Particles of dried or dehydrated liquid compositions can be prepared using conventional freeze-drying or lyophilization processes. This involves drying a larger volume of liquid composition, rather than drying individual droplets. Therefore, conventional methods result in the formation of a solid block or cake, which can then be broken down into particles within the desired size range. However, there are disadvantages associated with particles formed in this manner. For example, the cake formed by drying the liquid composition may be unevenly dried, and the particles formed by breaking down the block may not have a consistent composition, particularly regarding water content. Furthermore, when the cake is broken down into particles, this produces particles of varying shapes and sizes. Selecting particles within a certain size range is possible, but this results in at least some of the dried material being discarded, which is undesirable.

[0051] Furthermore, traditional freeze-drying or lyophilization methods used to form dried cakes can take several days and potentially up to two weeks. Faster and more efficient freeze-drying or lyophilization processes would be advantageous, and droplet drying to form shaped granules could significantly reduce the required drying time, for example, to less than a week and possibly as short as four days.

[0052] Careful formulation of liquid compositions also significantly affects freeze-drying time, as different liquid compositions have different critical temperatures. They must be freeze-dried below these critical temperatures to avoid structural changes and undesirable "swelling" due to formulation collapse. Higher freeze-drying temperatures result in shorter drying times.

[0053] Since the materials used for drying and molding granules can be highly hygroscopic, it is desirable to utilize the granules without further processing steps, as further processing steps may expose the granules to moisture and thus increase their moisture content, which can lead to a deterioration in workability, stability, and shelf life.

[0054] Indeed, the molded granules disclosed herein exhibit excellent physical stability and shelf life, and they can be easily transported and stored. In some embodiments, the granules can be stored at a storage temperature ranging from 0 to 35°C. In some embodiments, the granules can be stored at a relative humidity of up to about 30%.

[0055] Another advantage of dried shaped pellets is that they can be used directly in a variety of products without further processing after drying. For example, shaped pellets can be used as solid aerosol generating materials in combustible or non-combustible aerosol delivery systems, such as heated tobacco products (THP) or blending systems. They can also be used in aerosol-free delivery systems, such as systems that deliver at least one substance to a user via the mouth, nose, transdermis, or another method that does not require aerosol formation.

[0056] According to one aspect of the invention, each molded particle comprises a dried molding portion of a liquid composition containing plant extracts, such as tobacco extract. Therefore, the particles may contain one or more active substances and / or flavorings, and in at least some embodiments, these active substances and / or flavoring substances will be derived from the plant extracts. For example, in some embodiments, the particles contain one or more volatile or semi-volatile components derived from the plant extracts. These, in turn, may have already been derived from plant materials used to prepare the plant extracts. In other embodiments, these components may have been added to the liquid plant extract.

[0057] Liquid composition

[0058] The liquid composition contains plant extracts. In some embodiments, the liquid composition consists of plant extracts.

[0059] In some embodiments, the plant extract is a liquid plant extract. This type of extract is formed by contacting plant material with a solvent and then separating the solvent and any dissolved components from the solid plant material (also known as solid plant residue). A suitable solvent should be selected based on the components to be extracted from the plant material.

[0060] As used herein, the term "botanical" includes any material derived from a plant, including but not limited to extracts, leaves, bark, fibers, stems, roots, seeds, flowers, fruits, pollen, pods, shells, etc. Alternatively, the material may include naturally occurring or synthetically obtained active compounds from plants. The material may be in the form of liquid, solid, powder, dust, crushed particles, granules, pellets, fragments, strips, sheets, etc. Exemplary plants include tobacco, eucalyptus, star anise, hemp, cocoa, fennel, lemongrass, peppermint, spearmint, rooibos tea, chamomile, flax, ginger, ginkgo, hazelnut, hibiscus, bay leaf, licorice extract, matcha, mate, orange peel, papaya, rose, sage, tea such as green or black tea, thyme, clove, cinnamon, coffee, star anise, basil, bay leaf, cardamom, and coriander. Coriander, cumin, nutmeg, oregano, red chili pepper, rosemary, saffron, lavender, lemon peel, mint, juniper, elderflower, vanilla, holly, perilla, turmeric, turmeric root, sandalwood, coriander leaf, bergamot, orange blossom, myrtle, blackcurrant, valerian, pimento, mace, damien, marjoram, olive, lemon balm, lemon basil, chives, caraway, verbena, tarragon, geranium, mulberry, ginseng, theanine, theophylline, maca, ashwagandha, guarana, chlorophyll, baobab, or any combination thereof. Mint can be selected from the following varieties: wild mint (Mentha Arventis), cultivated mint variety (Mentha cv), Nile peppermint (Mentha niliaca), peppermint (Mentha piperita), citrus mint cultivar (Mentha piperita citrata cv), peppermint cultivar (Mentha piperita cv), spicy mint (Mentha spicata crispa), heart-shaped mint (Mentha cardifolia), long-leaved mint (Mentha longifolia), pineapple mint (Mentha suaveolens variegata), lip mint (Mentha pulegium), spearmint cultivar (Mentha spicata cv), and apple mint (Mentha suaveolens).

[0061] In some embodiments, the liquid composition contains a tobacco extract. In some embodiments, the liquid composition consists of a tobacco extract.

[0062] In some embodiments, the tobacco extract is a liquid tobacco extract. This extract is formed by contacting tobacco material with a solvent and then separating the solvent and any dissolved tobacco components from the solid tobacco material (also known as solid tobacco residue).

[0063] In some embodiments, the liquid tobacco extract is an aqueous extract. That is, the extract is formed by contacting tobacco material with an aqueous solvent. This produces a liquid extract and extracted solid tobacco material. The liquid extract may be at least partially separated from the solid tobacco material before forming the liquid composition. In some embodiments, the tobacco extract is used directly in the liquid composition or incorporated into the liquid composition.

[0064] Liquid tobacco extracts can be extracts from any type of tobacco and any part of the tobacco plant, including tobacco leaves, stems, stalks, veins, scraps, and short segments, or mixtures of two or more thereof. Suitable tobacco extracts or materials include the following types: Virginia or flue-cured tobacco, Burley tobacco, Oriental tobacco, or blends of tobacco materials, optionally including those listed herein. The tobacco can be expanded, such as dry ice expanded tobacco (DIET), or processed by any other means. In some embodiments, the tobacco material can be reconstituted tobacco material. The tobacco can be pre-processed or unprocessed, and can be, for example, solid stems (SS); chopped dried stems (SDS); steam-treated stems (STS); or any combination thereof. The tobacco material can be fermented, cured, uncured, roasted, or otherwise pre-treated.

[0065] In some embodiments, the tobacco extract has a solids content of about 40 to about 65 wt%, about 45 to about 65 wt%, or about 40 to about 60 wt% (based on wet weight). In some embodiments, the water content of the tobacco extract is about 35 wt% to about 65 wt%, or about 35 to about 55 wt% (based on wet weight). In some embodiments, the nicotine content of the tobacco extract is about 1 wt% to about 5 wt% (based on wet weight).

[0066] The liquid composition may be in the form of a slurry, suspension, emulsion, or solution. The liquid composition may contain plant extracts and other solvent components. The solvent components may include water. When other components are to be included in the dried material, these other components may be added alone or together with water. In some embodiments, the liquid composition may contain about 30 to about 70% v / v of plant extract, about 40 to about 60% v / v of plant extract, or about 50% v / v of plant extract.

[0067] Based on wet weight, the water content of the liquid composition may be at least about 20 wt%, at least about 30 wt%, at least about 40 wt%, at least about 50 wt%, at least about 60 wt%, at least about 70 wt%, at least about 80 wt%, or at least about 90 wt%. Additionally or alternatively, based on wet weight, the water content of the liquid composition may be at most about 95 wt%, at most about 90 wt%, at most about 85 wt%, at most about 80 wt%, at most about 75 wt%, at most about 70 wt%, at most about 65 wt%, at most about 60 wt%, at most about 55 wt%, or at most about 50 wt%. In some embodiments, based on wet weight, the water content of the liquid composition is from about 45 to about 90 wt%, or from about 55 to about 85 wt%.

[0068] The liquid composition may contain at least about 10 wt%, at least about 20 wt%, at least about 30 wt%, at least about 35 wt%, at least about 40 wt%, at least about 45 wt%, at least about 50 wt%, or at least about 55 wt% of tobacco solids (based on wet weight). Alternatively or additionally, the liquid composition may contain up to about 70 wt%, up to about 65 wt%, up to about 60 wt%, up to about 55 wt%, or up to about 50 wt% of tobacco solids (based on wet weight). In some embodiments, the liquid tobacco extract and / or the liquid composition contains about 10 wt% to about 65 wt% of tobacco solids (based on wet weight), or about 25 wt% to about 45 wt%.

[0069] In some embodiments, the liquid composition contains at least about 10 wt%, about 20 wt%, at least about 30 wt%, at least about 40 wt%, at least about 50 wt%, at least about 60 wt%, at least about 70 wt%, at least about 80 wt%, or at least about 90 wt% of tobacco extract (based on wet weight). Alternatively or additionally, the liquid composition contains up to about 99 wt%, up to about 90 wt%, up to about 80 wt%, up to about 70 wt%, or up to about 60 wt% of tobacco extract (based on wet weight). In some embodiments, the liquid composition contains about 40 to about 60 wt% of tobacco extract, or about 50 wt% of tobacco extract (based on wet weight).

[0070] In some embodiments, the liquid composition contains an active substance. The active substance used herein may be a physiologically active material, which is a material designed to achieve or enhance a physiological response.

[0071] In some embodiments, the active ingredient is derived from plant extracts. For example, in some embodiments, the active ingredient is nicotine derived from tobacco extracts.

[0072] Alternatively or additionally, the liquid composition may contain an active substance that is not derived from a plant extract. Suitable active substances may be selected from nutritional supplements, nootropics, and psychoactive substances. The active substance may be naturally occurring or synthetically obtained. The active substance may contain, for example, caffeine, taurine, caffeine, vitamins (such as B6 or B12 or C), melatonin, or components, derivatives, or combinations thereof. The active substance may contain one or more components, derivatives, or extracts of tobacco or another plant.

[0073] In some embodiments, the active ingredient may include nicotine derived from tobacco extracts, as well as additionally added nicotine or other active ingredients mentioned herein. In some embodiments, the active ingredient includes caffeine, melatonin, or vitamin B12.

[0074] In some embodiments, the liquid composition contains extracts from other plant sources in addition to tobacco extract.

[0075] In some embodiments, the plant extract is concentrated before being included in the liquid composition. This may make the drying step more efficient, for example, requiring less energy. Furthermore, this can help provide a liquid composition suitable for both the forming portion involving the liquid formation and the process of drying it to form shaped granules.

[0076] In some embodiments, the liquid composition contains one or more aerosol-forming agent materials.

[0077] Aerosol-forming agent materials may contain one or more components capable of forming aerosols. Aerosol-forming agent materials may be, for example, polyol aerosol generators or non-polyol aerosol generators. They may be solid or liquid at room temperature, but are preferably liquid at room temperature. In some embodiments, aerosol-forming agent materials may include one or more of the following: glycerol, propylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, 1,3-butanediol, erythritol, meso-erythritol, ethyl vanillate, ethyl laurate, diethyl octanoate, triethyl citrate, triacetin, a mixture of diacetins, benzyl benzoate, benzyl phenylacetate, glyceryl tribocate, lauryl acetate, lauric acid, myristic acid, and propylene carbonate.

[0078] In some embodiments, the aerosol-forming agent material comprises one or more polyols, such as propylene glycol, triethylene glycol, 1,3-butanediol, and glycerol; esters of polyols, such as glycerol monoacetate, glycerol diacetate, or glycerol triacetate; and / or aliphatic esters of mono-, di-, or polycarboxylic acids, such as dimethyl dodecanoate and dimethyl tetradecanoate. In some embodiments, the aerosol-forming agent material comprises one or more compounds selected from erythritol, propylene glycol, glycerol, vegetative glycerol (VG), triacetin, sorbitol, and xylitol. In some embodiments, the aerosol-forming agent material comprises glycerol, is substantially composed of glycerol, or is composed of glycerol. In a preferred embodiment, the aerosol-forming agent material is composed of glycerol.

[0079] Combinations of aerosol-forming agent materials can be used in equal or different proportions. Aerosol-forming agent materials can also be used as plasticizers.

[0080] In some embodiments, the liquid composition contains at least about 1% v / v, at least about 5% v / v, or at least about 10% v / v of aerosol-forming agent material. Alternatively or additionally, the liquid composition may contain up to about 20% v / v, up to about 15% v / v, up to about 10% v / v, or up to about 5% v / v of aerosol-forming agent material.

[0081] In embodiments of the invention where the aerosol-forming material is glycerol, the dried shaped particles may contain at least about 5 wt%, at least about 10 wt%, or at least about 12 wt% of the aerosol-forming agent material (based on dry weight). Alternatively or additionally, the aerosol-forming material may contain up to about 20 wt%, at most about 15 wt%, or at most about 20 wt% of glycerol (based on dry weight).

[0082] The amount of glycerol in the liquid composition and thus in the dried and shaped granules is important because it serves as both an aerosol-forming agent and a plasticizer. It is also important to remember that glycerol has antifreeze properties.

[0083] While it is desirable to contain sufficient glycerol to provide consumers with a adequate and pleasant aerosol, a balance needs to be struck, as excessive glycerol can adversely affect the freeze-drying process. If the glycerol concentration in the liquid composition is too high, it lowers the collapse temperature of the formulation, meaning freeze-drying must be carried out at a lower temperature, which increases the processing time required for drying and increases energy costs. If the collapse temperature of the formulation is low, structural changes occur. For example, this may involve the so-called "boiling" of the formulation, which will cause the product to collapse and a significant expansion of the dried particles will be observed. Therefore, freeze-drying must be carried out at a temperature below the collapse temperature of the formulation, and preferably about 2 to 7°C lower than the collapse temperature.

[0084] In some embodiments, the amount of glycerol contained in the liquid composition is no more than 5% v / v and can be as low as 0%.

[0085] In some embodiments, the liquid composition further contains one or more excipients.

[0086] The inventors have discovered that the presence of excipients can be important for the stability of liquid compositions during freeze-drying, particularly when the liquid composition contains glycerol as an aerosol-forming agent. This is likely because excipients increase the collapse temperature of the formulation. Indeed, experiments have shown that drying a liquid composition containing tobacco extract and glycerol but without excipients can lead to the undesirable structural changes discussed above during freeze-drying. They observed some “swelling” or significant expansion of the droplets during drying, indicating “boiling” of the liquid composition. Conversely, no such change was observed during droplet drying after adding excipients such as dextran (e.g., dextran 70K). Instead, uniformly sized beads formed, showing a slight shrinkage compared to the size of the frozen droplets before freeze-drying.

[0087] Suitable excipients include mannitol, sucrose, trehalose, lactose, sorbitol, raffinose, maltose, dextran 10, dextran 70, dextran 90, maltodextrin, gelatin, agar, cyclodextrin, PEG 2000-6000, and (PVP 10k).

[0088] In some embodiments, the liquid composition contains about 1 to about 20 wt% of one or more excipients based on wet weight. In some embodiments, the liquid composition may contain at least about 1 wt%, at least about 2 wt%, at least about 5 wt%, at least about 8 wt%, or at least about 10 wt% of excipients based on wet weight. Alternatively or additionally, the liquid composition may contain up to about 20 wt%, up to about 15 wt%, or up to about 10 wt% of excipients based on wet weight.

[0089] In some embodiments, the liquid composition contains about 50 wt% tobacco extract, about 0 to about 10% v / v glycerol, and about 10 wt% excipients. The tobacco extract may contain about 55 to about 62 wt% tobacco solids.

[0090] In some embodiments, the liquid composition may contain an acid. The acid may be an organic acid. In some of these embodiments, the acid may be at least one of a monocarboxylic acid, a dicarboxylic acid, and a tricarboxylic acid. In some such embodiments, the acid may contain at least one carboxyl functional group. In some such embodiments, the acid may be at least one of an α-hydroxy acid, a carboxylic acid, a dicarboxylic acid, a tricarboxylic acid, and a keto acid. In some such embodiments, the acid may be an α-keto acid.

[0091] In some such embodiments, the acid may be at least one selected from succinic acid, lactic acid, benzoic acid, citric acid, tartaric acid, fumaric acid, levulinic acid, acetic acid, malic acid, formic acid, sorbic acid, benzoic acid, propionic acid, and pyruvic acid.

[0092] In other embodiments, the acid may be an inorganic acid. In some of these embodiments, the acid may be a mineral acid. In some such embodiments, the acid may be at least one selected from sulfuric acid, hydrochloric acid, boric acid, and phosphoric acid.

[0093] In some embodiments, the preferred acids are lactic acid and / or levulinic acid.

[0094] The presence of acids can be beneficial because they can stabilize soluble species in tobacco extracts. For example, the presence of acids can reduce or essentially prevent nicotine from evaporating from the liquid composition before or during freeze-drying and lyophilization, thereby reducing nicotine loss during manufacturing.

[0095] In some embodiments, the liquid composition contains about 1 to about 5 wt% of one or more acids based on wet weight.

[0096] In some embodiments, the liquid composition further contains one or more seasonings.

[0097] As used herein, the terms “seasoning” and “flavoring agent” refer to materials that, where permitted by local regulations, may be used in products to create a desired taste, aroma, or other sensory experience for adult consumers. These may include naturally occurring flavoring materials, plants, plant extracts, synthetic materials, or combinations thereof (e.g., tobacco, licorice root extract (licorice), hydrangea, eugenol, Japanese white magnolia leaf, chamomile, fenugreek, clove, maple, matcha, menthol, Japanese mint, star anise, cinnamon, turmeric, Indian spices, Asian spices, vanilla, deer antler velvet, cherry, berries, cranberries, blueberries, peaches, apples, oranges, mangoes, citrus fruits, lemons, limes, tropical fruits, papaya, rhubarb, grapes, durian, dragon fruit, cucumber, blueberries, mulberries, citrus fruits, Scotch whisky liqueur, bourbon whisky, Scotch whisky, whisky, gin, tequila, rum, spearmint, peppermint, lavender, aloe vera, cardamom). Celery, quinoa, nutmeg, sandalwood, bergamot, geranium, arabesque, naswar, areca nut, hookah, pine, honey essence, rose oil, vanilla, lemon oil, orange oil, neroli, cherry blossom, cinnamon, caraway, cognac, jasmine, ylang-ylang, sage, fennel, wasabi, allspice, ginger, coriander, coffee, hemp, peppermint oil from any species of peppermint, eucalyptus, star anise, Cocoa, lemongrass, rooibos tea, flax, ginkgo, hazelnut, hibiscus, bay leaf, lotus root, orange peel, rose, tea such as green or black tea, thyme, juniper, elderflower, basil, bay leaf, cumin, oregano, red pepper, rosemary, saffron, lemon peel, mint, perilla, turmeric, coriander leaf, myrtle, blackcurrant, valerian, bell pepper, nutmeg peel, damiana, marjoram, olive, lemon balm. This includes balm, lemon basil, chives, caraway, verbena, tarragon, limonene, thymol, camphene, flavor enhancers, bitter taste receptor blockers, sensory receptor activators or stimulants, sugars and / or sugar substitutes (e.g., sucralose, acesulfame potassium, aspartame, saccharin, cyclamate, lactose, sucrose, glucose, fructose, sorbitol or mannitol), and other additives such as charcoal, chlorophyll, minerals, botanicals, or breath fresheners. These can be imitations, synthetic or natural ingredients or blends thereof. They can be in any suitable form, such as liquids like oils or solids like powders.

[0098] In some embodiments, the flavoring agent includes menthol, spearmint, and / or peppermint. In some embodiments, the flavoring agent includes flavoring components of cucumber, blueberry, citrus fruits, and / or cranberry. In some embodiments, the flavoring agent includes eugenol. In some embodiments, the flavoring agent includes flavoring components extracted from tobacco.

[0099] In some embodiments, the seasoning may include sensory agents designed to achieve somatosensory sensations that are typically chemically induced and perceived by stimulation of the fifth cranial nerve (trigeminal nerve) in addition to or in lieu of aroma or taste nerves, and these may include agents that provide heating, cooling, tingling, or numbing effects. Suitable heat-acting agents may be, but are not limited to, vanillyl ethyl ether, and suitable coolants may be, but are not limited to, eucalyptol and WS-3.

[0100] In some embodiments, the liquid composition contains about 0.1 to about 5 wt%, or about 1 to about 2 wt%, of one or more seasonings based on wet weight.

[0101] When the liquid composition contains hydrophobic flavorings, it may also need to contain surfactants or emulsifiers to allow the formation of stable oil-in-water emulsions. Suitable surfactants include, for example, fatty acid esters containing polyoxyethylene sorbitol (Tween) or sorbitol (Span), or lecithin.

[0102] Manufacture of shaped particles in the form of beads

[0103] To form the molded particles of the present invention in the form of beads, droplets of a liquid composition containing plant extracts are freeze-dried. In order to enable the liquid to be freeze-dried in the form of droplets, the liquid composition is first dispensed into a series of droplets, which are then rapidly pre-frozen (also referred to herein as “quick-freezing”) by exposure to extreme cold.

[0104] In some embodiments, droplets of the liquid composition are dispensed into liquid nitrogen. When the droplets of the liquid composition are exposed to a temperature of around -196°C, they freeze very rapidly.

[0105] The size of the beads can be adjusted by changing the size of the distributed droplets.

[0106] In some embodiments, the volume of the formed droplet is from about 1 to about 50 µl. In some embodiments, the volume or average (average) volume of the droplet is at least about 1 µl, at least about 5 µl, at least about 10 µl, at least about 15 µl, at least about 20 µl, at least about 25 µl, at least about 30 µl, at least about 35 µl, or at least about 40 µl. Additionally or alternatively, in some embodiments, the volume or average (average) volume of the droplet is not greater than 50 µl, about 45 µl, about 40 µl, about 35 µl, about 30 µl, about 25 µl, about 20 µl, or not greater than about 15 µl.

[0107] In some implementations, the droplets are pre-frozen at atmospheric pressure.

[0108] Droplets of liquid compositions tend to expand during pre-freezing. Their size may increase by about 5% to about 10%. Some crystallization may also be observed in frozen droplets.

[0109] Once formed, droplets of the pre-frozen liquid composition are freeze-dried.

[0110] Freeze-drying process

[0111] The molded portion of the liquid composition is dried by freeze-drying. In the above embodiment, the molded portion may be a spherical shape, formed as a frozen droplet.

[0112] In other embodiments, a mold can be used to create a shaped portion of the liquid composition. In such embodiments, at least one surface of the created shape will be flat. The liquid composition can be added to the mold, and the mold can then be placed in a freeze dryer for direct freeze-drying. In other embodiments, the liquid in the mold can be frozen, for example, by flash freezing, and the frozen portion can then be freeze-dried.

[0113] The drying method for the molded portion of the dry liquid composition can be any suitable freeze-drying process using known small or large freeze-drying equipment.

[0114] Freeze-drying, also known as lyophilization or freeze-drying, is a process that freezes a liquid composition, lowers the temperature, and removes moisture by sublimation under reduced pressure. It is not desirable to be bound by any particular theory, but it is believed that the low processing temperature and rapid water loss through sublimation prevent changes in the structure, appearance, and properties of the liquid composition. This process preserves the structure of the liquid composition and reduces the loss and decomposition of volatile components such as nicotine and flavoring compounds.

[0115] Freeze-drying can be carried out at a temperature of about -35°C to about -50°C. Freeze-drying can be carried out at a pressure of about 30 to about 40 μbar.

[0116] The dried granules formed by freeze-drying have a lower water content than the shaped portion of the liquid composition. The residual moisture content of the dried granules can be reduced to less than about 15%, and can be from about 5% to about 14% or from about 7% to about 12%, as measured by gas chromatography-thermal conductivity detector (GC-TCD) or Karl Fischer measurement. This low moisture content helps to avoid or control a phenomenon known as "hot puff" that may be seen in aerosol generation systems such as heated tobacco products.

[0117] Drying the liquid composition to form dry shaped particles can result in a reduction of water content of at least about 50 wt%, about 60 wt%, about 70 wt%, about 80 wt%, about 90 wt%, about 95 wt%, or at least about 98 wt%.

[0118] In some embodiments, the shaped portion of the liquid composition is freeze-dried for a period of about 48 hours to about 120 hours. In some embodiments, the freeze-drying is carried out for a period of at least about 48, 50, 55, 60, 65, 70, 75, 80, 85, 90, or at least about 95 hours. Additionally or alternatively, the freeze-drying is carried out for a period of no longer than about 120, 110, 100, 95, 90, 85, 80, 75, 70, 65, or no longer than about 60 hours.

[0119] Secondary drying

[0120] In some implementations, the freeze-dried molded portion undergoes a secondary drying step.

[0121] The first drying step (drying the liquid composition by freeze-drying) removes unbound water from the liquid composition. An optional secondary drying step may be performed to remove chemically bound water, thereby further reducing the moisture content of the dried particles.

[0122] In some embodiments, the secondary drying step may include gradually raising the temperature of the freeze-dried shaped particles to about +15°C to about +25°C, for example, to about +20°C, and then holding the shaped particles at that temperature for a period of time. During the secondary drying step, the temperature maintained for the freeze-dried shaped particles must not exceed room temperature to avoid dispersing the desired volatile components retained by the pre-freezing and freeze-drying steps from the liquid composition.

[0123] In some implementations, the endpoint of the secondary drying can be determined using a vacuum gauge to determine when water removal ceases (i.e., the water release plateau). In some implementations, this can be measured by Karl Fischer analysis, which may occur when the moisture content is below approximately 10%.

[0124] In some implementations, the molded particles can be kept at elevated temperatures for a period of about 10 to about 25 hours.

[0125] Drying of shaped particles

[0126] Due to the manufacturing process discussed above, the molded particles formed by drying the molding portion of a liquid composition containing plant extracts have easily controllable size, shape, and composition.

[0127] The geometry of the molded particles will be influenced by the geometry of the molded portion of the dried liquid composition. This, in turn, can be controlled by the methods used to form the molded portion, such as using pre-frozen droplets or molds.

[0128] In addition, the freeze-drying process causes slight shrinkage of the molded portion. The observed shrinkage occurs due to the removal of water from the freeze droplets; therefore, the greater the water content in the liquid composition (and freeze droplets), the greater the shrinkage observed after drying. This shrinkage may result in a reduction in size or volume of approximately 5% to 10%. The specific degree of shrinkage will depend on the shape and size of the portion.

[0129] When the molding portion has been pre-frozen, this step may cause initial expansion as discussed above. Subsequent shrinkage during freeze-drying may result in a return to approximately the pre-frozen size.

[0130] In some embodiments, the molded particles can be beads that are typically spherical in shape. In some embodiments, the beads have a slightly contracted spherical shape, meaning they may have a slightly uneven surface morphology.

[0131] The diameter of the beads will be affected by the volume of the droplets formed by the liquid composition and the solid content in the liquid composition. Some shrinkage will be observed during the drying process relative to the size of the frozen droplets.

[0132] The manufacturing process means that the size of the dried beads can be very uniform. In some embodiments, at least about 90% of the dried beads have a diameter that differs from the mass median diameter of the population by no more than 5%. In some embodiments, at least about 95%, at least about 97%, at least about 98%, or at least about 99% of the dried beads have a diameter that differs from the mass median diameter of the population by no more than 5%.

[0133] In some implementations, the dried beads are free-flowing and non-sticky, which facilitates bead handling.

[0134] In some embodiments, the drying beads have a diameter ranging from about 2 mm to about 5 mm. Optionally, the diameter can be at least about 2 mm, at least about 2.5 mm, at least about 3 mm, at least about 3.5 mm, at least about 4 mm, or at least about 4.5 mm. Alternatively or additionally, the diameter is no greater than about 5 mm, no greater than about 4.5 mm, no greater than about 4 mm, no greater than about 3.5 mm, no greater than about 3 mm, or no greater than about 2.5 mm. In some embodiments, the drying beads have an average diameter of about 2.5 to about 3 mm.

[0135] Beads with smaller diameters have a larger surface area to volume ratio, and therefore can exhibit faster component release compared to beads with larger diameters.

[0136] In some implementations, the size of the dried beads is selected to provide the desired release profile of one or more components. Generally, beads with smaller diameters or sizes release components more quickly and over shorter periods of time during use. Beads with larger diameters or sizes release components more gradually and over longer periods of time. In some implementations, beads of different sizes can be selected and combined to provide a release profile that starts quickly at the beginning of use and continues throughout an extended period of use.

[0137] In some embodiments, it may be desirable for the beads to have an average particle size or diameter of no more than about 5 mm, no more than 4 mm, no more than about 3 mm, or no more than about 2 mm when measured by sieving. In some embodiments, the beads have a diameter of about 2 to about 3 mm. This can be evaluated by sieving or by measuring using a QuickScope™ instrument to approximate a generally spherical diameter.

[0138] In some embodiments, the dried beads have a diameter of about 0.005 to about 0.02 cm. 3 The volume within the specified range. In some embodiments, the dried beads have an average volume of at least about 0.008 cm³. 3 At least approximately 0.009 cm 3 At least approximately 0.01cm 3 And / or the average volume is not greater than about 0.015 cm³. 3 Not larger than approximately 0.014 cm 3 Not larger than approximately 0.013 cm 3 or no larger than approximately 0.012 cm 3 .

[0139] In some embodiments, the dried shaped granules have a density of about 0.5 to about 1.5 g / cm³. 3 The density is within a certain range. In some embodiments, the molded particles have an average density of at least about 0.5 g / cm³. 3 At least approximately 0.6 g / cm 3 At least approximately 0.7 g / cm³ 3 and / or average density not greater than about 1.5 g / cm³ 3 Not greater than approximately 1.4 g / cm³ 3 Not greater than approximately 1.3 g / cm³ 3 Not greater than approximately 1.2 g / cm³ 3 or not greater than about 1.1 g / cm 3 .

[0140] In some embodiments, the dried shaped particles have a flat shape, such as a thin strip or a disc. In some embodiments, the flat shape has a thickness of about 0.05 mm to about 1 mm. In some embodiments, the thickness of the flat shape is at least about 0.05 mm, at least about 0.06 mm, at least about 0.07 mm, at least about 0.08 mm, at least about 0.09 mm, at least about 0.1 mm, at least about 0.15 mm, at least about 0.2 mm, at least about 0.25 mm, at least about 0.3 mm, at least about 0.4 mm, at least about 0.5 mm, at least about 0.6 mm, at least about 0.7 mm, at least about 0.8 mm, or at least about 0.9 mm. Alternatively or additionally, the thickness of the flat shape is not greater than about 1 mm, not greater than about 0.9 mm, not greater than about 0.8 mm, not greater than about 0.7 mm, not greater than about 0.6 mm, not greater than about 0.5 mm, not greater than about 0.45 mm, not greater than about 0.4 mm, not greater than about 0.35 mm, not greater than about 0.3 mm, not greater than about 0.25 mm, not greater than about 0.2 mm, not greater than about 0.15 mm, not greater than about 0.1 mm, not greater than about 0.09 mm, not greater than about 0.08 mm, not greater than about 0.07 mm, or not greater than about 0.06 mm.

[0141] In some embodiments, the flat shape matches the shape of shredded tobacco, for example having a width of about 0.8 to about 1.2 mm, a length of about 10 to about 40 mm, and a thickness of about 0.06 to about 0.2 mm.

[0142] The chemical composition of the dried granules will be controlled by the chemical composition of the liquid composition. The drying process is selected to mitigate or prevent the loss of desired components in the liquid composition, including, in particular, the loss of plant extract components. When the plant extract is a tobacco extract, it is desirable to retain tobacco components such as nicotine and volatile or semi-volatile flavorings and aromas. In some embodiments, the drying process essentially removes only water from the liquid composition. In other embodiments, some nicotine and / or glycerin may also be lost during the drying process, as they are both water-soluble.

[0143] In some embodiments, the dried shaped particles comprise dried plant extracts, such as dried tobacco extract. Optionally, the shaped particles may further comprise an aerosol-forming agent material. In some embodiments, the shaped particles also comprise excipients.

[0144] In some embodiments, the dried granules comprise about 45 to about 100% dried tobacco extract by weight. For example, the granules comprise at least about 50 wt%, at least about 55 wt%, at least about 60 wt%, at least about 65 wt%, at least about 70 wt%, at least about 75 wt%, at least about 80 wt%, at least about 85 wt%, or at least about 90 wt% of tobacco extract (based on dry weight). Alternatively or additionally, the dried granules comprise up to about 99 wt%, up to about 95 wt%, up to about 90 wt%, up to about 85 wt%, or up to about 80 wt% of tobacco extract (based on dry weight). In some embodiments, the dried granules comprise about 55 to about 85 wt% or about 50 to about 80 wt% of dried tobacco extract (based on dry weight).

[0145] In some implementations, the amount of tobacco extract included in the dried granules is as high as possible to provide as much nicotine and tobacco-derived flavoring and aroma as possible per unit weight of material. This high concentration of tobacco components will affect the weight and volume of the material that needs to be transported, stored, and incorporated into the final product.

[0146] In some implementations, the dried shaped granules may contain about 3-6 wt% nicotine derived from tobacco extract (based on dry weight). If additional nicotine is added, the total nicotine content of the granules may increase, for example, up to about 10 wt%.

[0147] In some embodiments, the dried shaped granules have a residual moisture content of greater than 7% and not more than 12%, or not more than 10%.

[0148] The water content of the molded granules described herein can vary depending on, for example, the temperature, pressure, and humidity conditions used to maintain the granules. The water content can be determined by Karl Fischer analysis or by gas chromatography-thermal conductivity detector (GC-TCD), as is known to those skilled in the art.

[0149] After manufacturing the dried granules, it may be desirable to store them in a controlled, dry environment to reduce the likelihood of the granules absorbing moisture from their surroundings. Ideally, the dried granules will be protected from moisture until they are used by consumers.

[0150] In some embodiments, the dried shaped granules comprise about 0.1 to about 30% by weight of aerosol-forming agent material. In some embodiments, the amount of aerosol-forming agent material in the dried granules is about 1 to about 25% by weight (based on dry weight), about 5 to about 20%, or about 5 to about 15% by weight.

[0151] Aerosol-forming agents can be included in dried, molded granules intended for use as aerosol-generating materials. When the dried granules containing the aerosol-forming agent material are heated, vapors and / or aerosols with desired properties can be formed. Furthermore, the aerosol-forming agent material can promote and control the release of plant components from the dried granules.

[0152] Aerosol-forming materials (such as glycerin and other materials mentioned herein) act as humectants and thus facilitate the retention and absorption of moisture by dried granules. Higher moisture content in dried granules can cause them to become sticky or viscous, making them more difficult to handle. The performance of dried granules in delivering components can be compromised by the additional moisture content and poorer handleability. Furthermore, it is wasteful to spend time and effort drying granules only to allow them to absorb moisture before use.

[0153] Furthermore, as discussed above and in the examples, it has been found that the amount of aerosol-forming agent material affects the outcome of the drying process and the optimal freeze-drying conditions. When the liquid composition contains a larger amount of aerosol-forming agent material, more frequent breakage of the dried particles is observed, resulting in particles of unpredictable size and shape.

[0154] Finally, it is recommended that at least some of the aerosol-forming materials (such as glycerol) included in the molded granules also act as antifreeze agents. Therefore, these materials will affect how the liquid composition behaves when exposed to freezing temperatures during the pre-freezing and freeze-drying steps. Thus, the amount of such agents must be selected to ensure that the drying process is not adversely affected. In particular, it is important that the process produces a consistent and predictable product.

[0155] In some embodiments, the dried shaped granules contain about 0.1 to about 25% by weight of excipients. In some embodiments, the amount of excipients in the dried granules is about 5 to about 20% by weight (based on dry weight).

[0156] Excipients are included in the dried shaped granules to stabilize the liquid composition during freeze-drying. As discussed in the examples, the presence and amount of excipients have been found to affect the outcome of the drying process. The liquid composition needs to be freeze-dried below its collapse temperature. The presence of excipients can increase the collapse temperature of the liquid composition, thus allowing freeze-drying at higher temperatures without increasing the risk of product collapse. This can lead to "bulking," producing large, bulging particles with properties very different from unbulked particles, resulting in significantly poorer product quality.

[0157] The dried shaped granules disclosed herein can be used in a variety of different delivery systems to deliver components of tobacco extract to users.

[0158] As used herein, the term "delivery system" is intended to cover systems that deliver at least one substance to a user, and includes: Combustible aerosol supply systems, such as cigarettes, cigarettes, cigars, and tobacco for pipes or for rolling or making cigarettes (whether based on tobacco, tobacco derivatives, expanded tobacco, reconstituted tobacco, tobacco substitutes, or other smokeable materials). Non-flammable aerosol supply systems that release compounds from aerosol-generating materials without burning the materials themselves, such as electronic cigarettes, heated tobacco products, and mixing systems that use combinations of aerosol-generating materials to produce aerosols; and A non-aerosol delivery system that delivers at least one substance to a user via the mouth, nose, transdermis, or another method that does not form an aerosol, including but not limited to lozenges, gum, patches, articles containing inhalable powder, and oral products such as oral tobacco including snuff or wet snuff, wherein at least one substance may or may not contain nicotine.

[0159] In some implementations, dried shaped granules can be used in a delivery system without significant further processing. For example, it may not be necessary to adjust or select the particle size.

[0160] Aerosol generating material

[0161] The dried, molded granules of this invention can be used as aerosol-generating materials. An aerosol-generating material is a material capable of producing aerosols, for example, when heated, radiated, or powered in any other way.

[0162] In some embodiments, the aerosol generating material is used in a "non-flammable" aerosol supply system. According to this disclosure, a "non-flammable" aerosol supply system is a system in which the aerosol generating material, which is a component of the aerosol supply system (or its components), does not burn or ignite to facilitate the delivery of at least one substance to a user.

[0163] In some implementations, the delivery system is a non-flammable aerosol supply system, such as a powered (electric) non-flammable aerosol supply system.

[0164] In some implementations, the non-flammable aerosol supply system is an electronic cigarette, also known as a vaping device or electronic nicotine delivery system (END), although it should be noted that the presence of nicotine in the aerosol generating material is not necessary.

[0165] In some implementations, the non-flammable aerosol supply system is an aerosol-generating material heating system, also known as a heated non-flammable system. An example of such a system is a tobacco heating system.

[0166] In some embodiments, the non-flammable aerosol supply system is a mixing system that uses a combination of aerosol-generating materials to generate aerosols, wherein one or more aerosol-generating materials can be heated. Each aerosol-generating material can be in, for example, solid, liquid, or gel form, and may or may not contain nicotine. In some embodiments, the mixing system comprises liquid or gel aerosol-generating materials and solid aerosol-generating materials. Solid aerosol-generating materials may comprise, for example, tobacco or non-tobacco products.

[0167] Typically, a non-flammable aerosol supply system may include a non-flammable aerosol supply device and consumables used in conjunction with the non-flammable aerosol supply device.

[0168] In some embodiments, this disclosure relates to consumables comprising aerosol-generating materials and configured for use with a non-flammable aerosol supply device. Throughout this disclosure, these consumables are sometimes referred to as articles.

[0169] In some embodiments, a non-flammable aerosol supply system, such as its non-flammable aerosol supply device, may include a power source and a controller. The power source may be, for example, an electrical power source or an exothermic power source. In some embodiments, the exothermic power source includes a carbon substrate that can be powered to distribute power in the form of heat to the aerosol-generating material or to a heat transfer material adjacent to the exothermic power source.

[0170] In some implementations, a non-flammable aerosol supply system may include an area for receiving consumables, an aerosol generator, an aerosol generation area, a housing, a mouthpiece, a filter, and / or an aerosol modifier.

[0171] In some embodiments, consumables used with the non-flammable aerosol supply device may include aerosol generating material, aerosol generating material storage area, aerosol generating material transfer assembly, aerosol generator, aerosol generating area, housing, wrapper, filter, mouthpiece and / or aerosol modifier.

[0172] The dried shaped granules disclosed herein provide aerosol-generating materials that are stable within a certain temperature range, allowing for storage and / or transportation over extended periods without deterioration of aerosol properties. The low water content also inhibits microbial growth.

[0173] In some embodiments, the consumable comprises about 50 to about 250 mg of molded particles, about 50 to about 200 mg, about 50 to about 150 mg, or about 100 mg of molded particles.

[0174] In some implementations, the dried shaped particles are the only aerosol generating material used, or they are the only solid aerosol generating material used to generate aerosols.

[0175] In other embodiments, the dried shaped particles of the present invention can be combined with one or more other aerosol-generating materials. For example, the dried shaped particles can be combined with aerosol-generating materials comprising tobacco materials or other plant or plant materials. Different aerosol-generating materials can be provided individually or together, for example, as mixtures or blends.

[0176] Aerosol-generating materials may contain nicotine.

[0177] Incorporation into an aerosol generating device

[0178] In some implementations, dried molded granules are provided as consumables.

[0179] Consumables are articles containing aerosol-generating materials, which are intended in whole or in part for consumption by a user during use. Consumables may include one or more other components, such as an aerosol-generating material storage area, an aerosol-generating material delivery assembly, an aerosol-generating area, a housing, packaging materials, a mouthpiece, a filter, and / or an aerosol modifier. Consumables may also include an aerosol generator, such as a heater, which generates heat during use to cause the aerosol-generating material to produce an aerosol. The heater may, for example, include a combustible material, a material that can be heated by electrical conduction, or a susceptor. Consumables can be of any shape or size suitable for an aerosol supply device. In some embodiments, the consumable is rod-shaped.

[0180] In some embodiments, a group of dried shaped particles is provided in an aerosol generating device, such as a heated tobacco product (THP) or a hybrid e-cigarette product. Advantageously, the dried shaped particles can be used directly as a solid substrate and can be directly heated to provide an inhalable aerosol without ignition. Heating the particles can aerosolize the components of the dried particles (e.g., glycerin, nicotine, and / or tobacco flavorings). The dried shaped particles and / or consumables can be stored under reduced humidity conditions, such as humidity below about 30%, before use.

[0181] An added benefit of using dried shaped granules directly as a solid substrate is that the low water content reduces problems associated with “hot smoke” known in the art.

[0182] Figure 1 This is a side cross-sectional view of a consumable or article 1 used in an aerosol delivery system. Article 1 includes a mouthpiece section 2 and an aerosol generation section 3.

[0183] The aerosol generating section 3 is in the form of a cylindrical rod and contains an aerosol generating material 4, which comprises the group of dried-formed particles disclosed herein. For example, the dried-formed particles can be any particles or beads discussed herein.

[0184] Although the rod form has been described above, the aerosol generating section 3 may be provided in other forms, such as a plug, pouch, or package of material within the article.

[0185] In an example embodiment, the mouthpiece segment 2 includes a material body 5, such as fibers or filament bundles.

[0186] The rod-shaped consumable 1 further includes packaging material 6, such as paper packaging material, surrounding the mouthpiece section 2 and the aerosol generating section 3.

[0187] Figure 2 An example of the non-flammable aerosol supply device 100 described herein is shown, which is used to generate an aerosol from an aerosol generating medium, such as the aerosol generating material of consumable 110. In summary, device 100 can be used to heat a replaceable article 110 containing an aerosol generating medium, for example... Figure 1 The article 1 shown or otherwise described herein is used to generate an aerosol or other inhalable medium for inhalation by the user of device 100. Device 100 and replaceable article 110 together form a system.

[0188] The device 100 includes a housing 102 (in the form of an outer casing) that surrounds and houses the various components of the device 100. The device 100 has an opening 104 at one end through which an article 110 can be inserted to be heated by a heating assembly. In use, the article 110 can be fully or partially inserted into the heating assembly, where it is heated by one or more components of the heater assembly.

[0189] The device 100 in this example includes a first end member 106, which includes a cap 108 movable relative to the first end member 106 to close the opening 104 when no article 110 is placed thereon. Figure 2 In the image, the lid 108 is shown in the open position; however, the lid 108 can be moved to the closed position. For example, a user can slide the lid 108 in the direction of arrow "B".

[0190] The device 100 may also include a user-operable control element 112, such as a button or switch, which operates the device 100 when pressed. For example, a user can turn on the device 100 by operating the switch 112.

[0191] Device 100 may also include electrical components, such as a receptacle / port 114, which can receive a cable to charge the battery of device 100. For example, receptacle 114 may be a charging port, such as a USB charging port.

[0192] Aerosol free delivery

[0193] In some embodiments, the delivery system is an aerosol-free delivery system that delivers at least one substance to a user via the mouth, nose, transdermis, or in another manner that does not form an aerosol. This includes, but is not limited to, lozenges, chewing gum, patches, articles containing inhalable powder, and oral products such as oral tobacco, including snuff or wet snuff, wherein at least one substance may or may not contain nicotine.

[0194] In some embodiments, dried shaped granules are packaged into sachets for oral administration. The dried shaped granules may be the only material included in the sachet, or they may be combined with other materials, including other sources of active substances and / or flavoring substances.

[0195] Figure 3 An example of a permeable pouch is shown. Pouch 21 comprises two porous material sheets 22. These sheets are fused or adhered along their edges to form a chamber in which a seasoning delivery and / or active substance delivery composition 23 is sealed. This seasoning delivery and / or active substance delivery composition comprises the dried-formed granules disclosed herein.

[0196] Because dried, molded granules provide a highly concentrated form of plant (e.g., tobacco) extracts, oral sachets can be very small while still delivering a greater physiological and sensory impact than regular oral sachets. This can be beneficial in terms of user comfort or product variability.

[0197] In some implementations, using polysaccharides (such as dextran) as excipients means that the dried shaped granules can be sweet when placed in the mouth. This reduces the need for including other or any additional sweeteners or flavorings.

[0198] Other possible aerosol-free delivery systems, including the dried molded granules disclosed herein, deliver the components to the user via oral, nasal, transdermal, or any other suitable route of administration. In some embodiments, the molded granules are incorporated into products selected from the group consisting of lozenges, chewing gum, patches, and inhalable powders.

[0199] Example

[0200] Example 1 - Nicotine retention

[0201] The nicotine content of the liquid composition and the dried beads after the freeze-drying process was calculated, thus providing an indication of the amount of nicotine retained after processing. The nicotine recovery rate of the dried aerosol-generating material, based on dry weight, is at least about 50 wt% compared to the virgin tobacco extract. The nicotine recovery rate of the dried aerosol-generating material, based on dry weight, can be at least about 55%, at least about 60%, at least about 75%, at least about 80%, or at least about 90% compared to the virgin tobacco extract.

[0202] Example 2 - Glycerol retention

[0203] The glycerol content of the precursor and the dried aerosol-generating material after the freeze-drying process was calculated, thus providing an indication of the amount of glycerol retained after processing. The glycerol recovery rate of the dried aerosol-generating material was at least about 50% compared to the precursor material. The glycerol recovery rate of the dried aerosol-generating material, based on dry weight, could be at least about 60%, at least about 70%, at least about 75%, at least about 80%, at least about 85%, at least about 90%, or at least about 95% compared to the precursor material.

[0204] Example 3

[0205] 1. Liquid composition

[0206] A series of liquid composition samples were prepared according to the compositions shown in Table 1 below.

[0207] A liquid aqueous tobacco extract was combined with an equal volume of a solvent containing an aqueous solution of an excipient and / or aerosol-forming agent. The excipient used was dextran 70. The aerosol-forming agent used was glycerol. The effects of this component on the process and product were observed using three different aqueous tobacco extracts.

[0208] Table 1

[0209] 2. Quick-freezing droplets

[0210] Droplets of approximately 20 µl were dispensed into vacuum flasks (Dewar flasks) containing liquid nitrogen. The frozen droplets formed from each sample were then transferred to individual vials at -50°C and atmospheric pressure. The frozen droplets were uniform in size and shape, although there were some variations in color. The frozen droplets were essentially spherical.

[0211] 3. Initial (freeze-drying) stage

[0212] The cryogenic liquid was freeze-dried for 5380 minutes at a temperature of -50°C and a pressure of 30 µbar.

[0213] 4. Secondary drying stage

[0214] Then, the temperature of the freeze-dried beads was adjusted to 20°C over a period of 140 minutes. The pressure was maintained at 30 µbar. Once the target temperature of 20°C was reached, the beads were held at that temperature and 30 µbar for another period of 1250 minutes.

[0215] Table 2 summarizes the properties of the obtained dried beads.

[0216] Table 2

[0217] The following conclusions can be drawn from the above comments.

[0218] The excipient dextran 70 was found to stabilize the liquid composition during drying and appeared to prevent the observed undesirable swelling (expansion). This phenomenon did not occur in all beads in this batch, but when the liquid composition did not contain the excipient, a portion of the dried material was unusable. The lack of the excipient also resulted in incomplete drying of sample 1.

[0219] Despite its antifreeze properties, the amount of glycerin contained appears to have little impact on the product's appearance and does not seem to adversely affect the drying process at -50°C.

[0220] Example 4

[0221] The effects of the inclusion of glycerol and excipients (dextran 70 in this case) on the collapse temperature of the formulation were evaluated, and the results are shown in Table 3.

[0222] Table 3

[0223] This data shows that the presence of glycerin lowers the collapse temperature. This means that formulations containing glycerin require freeze-drying at lower temperatures (and for longer periods).

[0224] The data also indicate that including dextran as an excipient increases the collapse temperature. This means that some of the effects of including glycerol in the liquid composition can be compensated for by including excipients. Furthermore, including excipients makes the freeze-drying process cheaper and faster because it increases the temperature at which the process can be carried out without the risk of formulation collapse and the unacceptable impact of such collapse on the resulting dried composition.

[0225] The various embodiments described herein are provided only to aid in understanding and teaching the claimed features. These embodiments are provided only as representative examples of implementation and are not exhaustive and / or exclusive. It should be understood that the advantages, implementations, examples, functions, features, structures and / or other aspects described herein should not be considered as limitations on the scope of the invention as defined by the claims or on the equivalents of the claims, and other embodiments can be utilized and modifications can be made without departing from the scope of the claimed invention. Various embodiments of the invention may suitably comprise, consist of, or substantially consist of suitable combinations of the disclosed elements, components, features, portions, steps, devices, etc., other than those specifically described herein. Furthermore, this disclosure may include other inventions not currently claimed but which may be claimed in the future.

Claims

1. Shaped particles, each shaped particle comprising a freeze-dried shaped portion of a liquid composition containing a plant extract.

2. The shaped particle of claim 1, wherein, The shaped particles comprise volatile and semi-volatile components of the plant extract.

3. The shaped particle of claim 1 or 2, wherein, The plant extract is a tobacco extract, and optionally an aqueous tobacco extract.

4. The shaped particles of any one of claims 1 to 3, the liquid composition further containing an aerosol-former material.

5. The shaped particle of claim 4, wherein, The aerosol-former material is glycerol.

6. The shaped particles of any one of claims 1 to 5, the liquid composition further containing an excipient.

7. The shaped particle of any one of claims 1 to 6, wherein, The excipient is dextran.

8. The shaped particles of any one of claims 1 to 7, comprising about 45% to about 100% by weight of dried plant extract (on a dry weight basis).

9. The shaped particles of any one of claims 1 to 8, comprising about 1% to about 20% by weight of aerosol-former material (on a dry weight basis).

10. The shaped particles of any one of claims 1 to 9, comprising about 0.1% to about 20% by weight of excipient (on a dry weight basis).

11. The shaped particle of any one of claims 1 to 10, wherein, The shaped particles are freeze-dried droplets of the liquid composition containing a plant extract.

12. The shaped particle of any one of claims 1 to 11, wherein, The shaped particles are spheroid beads.

13. The shaped particle of claim 12, wherein, At least 90% of the beads have a diameter that differs from the mass median diameter of the population by no more than 5%.

14. The shaped particle of claim 12 or 13, wherein, The beads have a diameter in the range of about 2 mm to about 5 mm.

15. The shaped particle of any one of claims 12 to 14, wherein, The beads have a volume of about 0.005 to about 0.02 cm 3 .

16. The shaped particle of any one of claims 1 to 15, wherein, The shaped particles have a density in the range of about 0.5 to about 1.5 g / cm 3 .

17. The shaped particle of any one of claims 1 to 11, wherein, The shaped particles are flat in shape, such as thin ribbons or discs.

18. The shaped particles of claim 17, having a thickness of about 0.05 mm to about 1 mm.

19. The shaped particles of any one of claims 1 to 18, having a residual moisture content of no more than about 12% or no more than about 10%, as measured by Karl Fischer analysis.

20. The shaped particles of claim 19, having a residual moisture content of at least 7%, as measured by Karl Fischer analysis.

21. A method of providing shaped particles, comprising: providing a portion of a liquid composition containing a plant extract in a mould; and freeze-drying the liquid composition in the mould.

22. A method of providing shaped particles, comprising: pre-freezing droplets of a liquid composition containing a plant extract; and freeze-drying the frozen droplets to form beads.

23. The method of claim 22, wherein, The droplets of the liquid composition containing a plant extract have a volume of about 1 μl to about 50 μl.

24. The method of claim 22 or 23, wherein, The droplets are pre-frozen by dispensing the droplets of the liquid composition into liquid nitrogen.

25. The method of claim 24, wherein, The droplets are pre-frozen at atmospheric pressure.

26. The method of claim 24 or 25, wherein, The droplets are instantaneously frozen upon contact with the liquid nitrogen.

27. The method of any one of claims 21 to 26, wherein, The freeze-drying is performed at a temperature of about -35 to about -50 °C.

28. The method of any one of claims 21 to 27, wherein, The freeze-drying is performed at a pressure of about 30 to about 40 μbar.

29. The method of any one of claims 21 to 28, wherein, The freeze-drying is performed for a period of about 48 hours to about 120 hours.

30. The method of any one of claims 21 to 29, comprising a secondary drying step.

31. The method of claim 30, wherein, The secondary drying step comprises raising the temperature of the freeze-dried shaped particles to a secondary drying temperature of no more than 20 °C.

32. The method of claim 31, wherein, The freeze-dried shaped particles are held at the secondary drying temperature for a period of from about 9 hours to about 24 hours.

33. The method of any one of claims 30-32, wherein, The secondary drying step is carried out at a pressure of from about 20 to about 30 μbar.

34. A non-combustible aerosol provision system comprising the shaped particles of any of claims 1 to 20.

35. A non-combustible aerosol provision system according to claim 34, wherein, The system is configured to heat the shaped particles to form a vapour and / or aerosol.

36. A non-combustible aerosol provision system according to claim 34 or 35, further comprising a further aerosol generating material which is to be heated to form an aerosol and / or vapour, optionally wherein the further aerosol generating material is a liquid.

37. An article for use in a non-combustible aerosol provision system comprising the shaped particles of any of claims 1 to 20.

38. An oral product comprising a permeable container enclosing the shaped particles of any of claims 1 to 20.

39. A method for providing the article of claim 37 or the oral product of claim 38, comprising: forming one or more shaped particles according to the method of any of claims 21 to 33; and placing the one or more shaped particles in a container.

40. Use of the shaped particles of any of claims 1 to 20 for generating an inhalable medium.

41. A shaped particle obtained or obtainable by the method of any of claims 21 to 33 for use in an aerosol provision system to generate an inhalable medium. ​

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