Dried shaped particles, method of manufacturing them, and uses thereof

Abstract

The 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 uses thereof.

Description

[0001] Dried shaped particles, method of manufacturing them, and uses thereof

[0002] Field

[0003] The 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 uses thereof.

[0004] Background

[0005] It is challenging to prepare a dry, solid material from liquid compositions comprising tobacco extracts whilst retaining desirable components including those that are volatile or semi-volatile. The dried material formed by conventional freeze-drying or lyophilisation methods will generally be formed as a solid mass or cake that is then broken down into particles of a desired size.

[0006] Summary

[0007] According to a first aspect of the invention there is provided shaped particle each comprising a freeze-dried shaped portion of a liquid composition comprising a botanical extract.

[0008] In some embodiments, the shaped particles comprise volatile and semi-volatile components of the botanical extract.

[0009] In some embodiments, the botanical extract is a tobacco extract and optionally an aqueous tobacco extract.

[0010] In some embodiments, the liquid composition further comprising an aerosol-former material. In some embodiments, the aerosol-former material is glycerol.

[0011] In some embodiments, the liquid composition further comprising an excipient. In some embodiments, the excipient is a dextran.

[0012] In some embodiments, the shaped particles comprise from about 45 to about 100% by weight dried botanical extract (on a dry weight basis).

[0013] In some embodiments, the shaped particles comprise from about 1 to about 20% by weight aerosol-former material (on a dry weight basis). In some embodiments, the shaped particles comprise from about 0.1 to about 20% by weight of an excipient (on a dry weight basis).

[0014] In some embodiments, the shaped particles are freeze-dried droplets of the liquid composition comprising a botanical extract.

[0015] In some embodiments, the shaped particles are spheroid beads.

[0016] In some embodiments, at least 90% of the beads have a diameter that varies by no more than 5% from the mass median diameter of the population.

[0017] In some embodiments, the beads have a diameter in the range of from about 2 mm to about 5 mm.

[0018] In some embodiments, the beads have a volume of from about 0.005 to about 0.02 cm3.

[0019] In some embodiments, the shaped particles have a density in the range of from about 0.5 to about 1.5 g / cm3.

[0020] In some embodiments, the shaped particles are flat shapes, such as thin strips or discs.

[0021] In some embodiments, the shaped particles have a thickness of from about 0.05 mm to about 1 mm.

[0022] 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 Fisher analysis.

[0023] In some embodiments, the residual moisture content is at least 7%, as measured by Karl Fisher analysis.

[0024] According to a second aspect of the invention there is provided a method of providing shaped particles, comprising : providing portions of a liquid composition comprising a botanical extract in a mould; and freeze-drying the liquid composition in the mould. In some embodiments, the method comprises: pre-freezing droplets of a liquid composition comprising a botanical extract; and freeze-drying the frozen droplets to form beads.

[0025] In some embodiments, the droplets of the liquid composition comprising a botanical extract have a volume of from about 1 pl to about 50 pl.

[0026] In some embodiments, the droplets are pre-frozen by dispensing droplets of the liquid composition into liquid nitrogen.

[0027] In some embodiments, the droplets are pre-frozen at atmospheric pressure.

[0028] In some embodiments, the droplets are frozen instantaneously on contact with the liquid nitrogen.

[0029] In some embodiments, the freeze-drying is carried out at a temperature of from about -35 to about -50°C

[0030] In some embodiments, the freeze-drying is carried out at a pressure of from about 30 to about 40 pbar.

[0031] In some embodiments, the freeze-drying is carried out for a period of from about 48 hours to about 120 hours.

[0032] In some embodiments, the method comprises a secondary drying step.

[0033] In some embodiments, the secondary drying step involves increasing the temperature of the freeze-dried shaped particles to a secondary drying temperature of no more than 20°C.

[0034] In some embodiments, the freeze-dried shaped particles are held at the secondary drying temperature for a period of from about 9 hours to about 24 hours.

[0035] In some embodiments, the secondary drying step is carried out at a pressure of from about 20 to about 30 pbar. According to a third aspect of the invention, there is provided a non-combustible aerosol-provision system comprising shaped particles according to the first aspect.

[0036] In some embodiments, the system is configured to heat the shaped particles to form a vapour and / or aerosol.

[0037] In some embodiments, the non-combustible aerosol-provision system comprises a further aerosol-generating material which is to be heated to form an aerosol and / or vapour. In some embodiments, the further aerosol-generating material is a liquid.

[0038] According to a fourth aspect of the invention, an article for use in a non-combustible aerosol-provision system is provided, comprising shaped particles according to the first aspect.

[0039] According to a fifth aspect of the invention, there is provided an oral product comprising a permeable container surrounding shaped particles according to the first aspect.

[0040] According to a sixth aspect, there is provided a method for providing an article according to the fourth aspect or an oral product according to the fifth aspect, comprising : forming one or more shaped particles according to a method according to the second aspect; and placing the one or more shaped particle in a container.

[0041] According to a seventh aspect, there is provided the use of a shaped particle as claimed in any one of claims 1 to 20 to generate an inhalable medium.

[0042] According to an eighth aspect, there is provided a shaped particle obtained or obtainable by a method according to the second aspect, for use in an aerosol provision system to generate an inhalable medium.

[0043] Brief Description of the Drawings

[0044] Embodiments of the invention will now be described, by way of example only, with reference to accompanying drawings, in which:

[0045] Figure 1 is a side-on cross-sectional view of a first embodiment of a consumable comprising aerosol generating material including dried shaped particles according to the invention. Figure 2 is a perspective illustration of a non-combustible aerosol provision device for generating aerosol from the aerosol-generating material of the consumable shown in Figure 1.

[0046] Figure 3 is schematic representation of a permeable container or pouch holding a population of dried shaped particles according to the invention.

[0047] Detailed Description

[0048] The present invention relates to a plurality or population of shaped particles, such as beads, that each comprise a dried or dehydrated shaped portion of a liquid composition comprising a botanical extract. For example, the botanical extract may be a tobacco extract.

[0049] The term "shaped" as used herein means that the particles have a controlled and predetermined shape. These particles are not, for example, formed by creating a larger dried mass which is then broken up into particles. Such a process would not provide particles of a controlled and predetermined shape. Instead, the liquid composition is dried in a preformed shape to form a shaped particle. As discussed below, there are different ways to achieve this.

[0050] As each shaped particle comprises a dried shaped portion of a liquid composition, a plurality or a population of these shaped particles have a number of beneficial properties. Firstly, the composition of each shaped particle may be accurately controlled. Secondly, the size and the shape or form of each particle may be accurately controlled. Thirdly, in some embodiments, the shaped particles can be free-flowing and easy to handle, store and process.

[0051] Significantly, the ability to manufacture shaped particles with a predictable composition, size and shape means that the particles may be used to provide an accurate and predictable delivery of components upon use. Further, a population of particles comprising a mixture of different particles (i.e., a mixture of particles with different properties) may be used to provide desired delivery profiles over a period of time.

[0052] The shaped particles according to the invention may be made by freeze drying a liquid composition in portions of the desired shape.

[0053] Particles of a dried or dehydrated liquid composition can be made using conventional freeze-drying or lyophilisation processes. This involves the drying of a larger volume of the liquid composition rather than the drying of individual droplets. Therefore, the conventional approach results in the formation of a solid mass or cake, which can then be broken down into particles of a desired size range. However, there are disadvantages associated with the particles formed in this way. For example, the cake formed by drying the liquid composition may not be uniformly dried and the particles formed by breaking up the mass may also not have a consistent composition, especially in terms of water content. Also, when the cake is broken into particles, this can result in particles of different shapes and sizes. Selection of particles within a certain size range is possible, but will result in at least some of the dried material being discarded, which is undesirable.

[0054] Further, traditional freeze-drying or lyophilisation methods used to form a dried cake can take several days and possibly up to two weeks. A faster and more efficient freeze-drying or lyophilisation process would be advantageous and the drying of liquid droplets to form shaped particles can significantly reduce the drying time required, for example down to less than week and possibly as little as 4 days.

[0055] Careful formulation of the liquid composition will also dramatically affect the freeze- drying time, as different liquid compositions have different critical temperatures below which they must be freeze dried to avoid structural changes and undesirable "puffing" as a result of formulation collapse. Higher freeze-drying temperatures result in shorter drying times.

[0056] As the material of the dried shaped particles can be very hygroscopic, it is desirable to be able to utilise the particles without further processing steps that could expose them to moisture and therefore increase their moisture content, which can lead to a deterioration in handleability, stability and shelf-life.

[0057] Indeed, the shaped particles disclosed herein exhibit excellent physical stability and shelf life, and they may be easily transported and stored. In some embodiments, the particles may be stored at temperatures in the range storage temperatures in the range 0-35°C. In some embodiments, the particles may be stored at a relative humidity of up to about 30%.

[0058] A yet further advantage of the dried shaped particles is that they may be directly used in a range of products without the need for further processing once dried. For example, the shaped particles may be used as a solid aerosol-generating material in combustible or non-combustible aerosol provision systems such as Tobacco Heating Products (THPs) or Hybrid systems. They may also be used in aerosol-free delivery systems such as those that deliver at least one substance to a user orally, nasally, transdermally or in another way without forming an aerosol.

[0059] The shaped particles according to an aspect of the present invention each comprise a dried shaped portion of a liquid composition comprising a botanical extract, such as a tobacco extract. Therefore, the particles may comprise one or more active substances and / or flavours and in at least some embodiments, these active and / or flavour substances will be derived from the botanical extract. For example, in some embodiments the particles comprise one or more volatile or semi-volatile components from the botanical extract. These, in turn, may have been derived from the botanical material used to prepare the botanical extract. In other embodiments, these components may have been added to the liquid botanical extract.

[0060] The liquid composition

[0061] The liquid composition comprises a botanical extract. In some embodiments, the liquid composition consists of the botanical extract.

[0062] In some embodiments, the botanical extract is a liquid botanical extract. Such an extract is formed by contacting botanical material with a solvent and then separating the solvent and any dissolved components from the solid botanical material (also referred to as the solid botanical residue). A suitable solvent should be selected based upon the components to be extracted from the botanical material.

[0063] As used herein, the term "botanical" includes any material derived from plants including, but not limited to, extracts, leaves, bark, fibres, stems, roots, seeds, flowers, fruits, pollen, husk, shells or the like. Alternatively, the material may comprise an active compound naturally existing in a botanical, obtained synthetically. The material may be in the form of liquid, solid, powder, dust, crushed particles, granules, pellets, shreds, strips, sheets, or the like. Example botanicals are tobacco, eucalyptus, star anise, hemp, cocoa, cannabis, fennel, lemongrass, peppermint, spearmint, rooibos, chamomile, flax, ginger, ginkgo biloba, hazel, hibiscus, laurel, licorice (liquorice), matcha, mate, orange skin, papaya, rose, sage, tea such as green tea or black tea, thyme, clove, cinnamon, coffee, aniseed (anise), basil, bay leaves, cardamom, coriander, cumin, nutmeg, oregano, paprika, rosemary, saffron, lavender, lemon peel, mint, juniper, elderflower, vanilla, Wintergreen, beefsteak plant, curcuma, turmeric, sandalwood, cilantro, bergamot, orange blossom, myrtle, cassis, valerian, pimento, mace, damien, marjoram, olive, lemon balm, lemon basil, chive, carvi, verbena, tarragon, geranium, mulberry, ginseng, theanine, theacrine, maca, ashwagandha, damiana, guarana, chlorophyll, baobab or any combination thereof. The mint may be chosen from the following mint varieties: Mentha Arventis, Mentha c.v., Mentha niliaca, Mentha piperita, Mentha piperita citrata c.v., Mentha piperita c.v., Mentha spicata crispa, Mentha cardifolia, Mentha longifolia, Mentha suaveolens variegata, Mentha pulegium, Mentha spicata c.v. and Mentha suaveolens

[0064] In some embodiments, the liquid composition comprises a tobacco extract. In some embodiments, the liquid composition consists of the tobacco extract.

[0065] In some embodiments, the tobacco extract is a liquid tobacco extract. Such an 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 referred to as the solid tobacco residue).

[0066] 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 creates a liquid extract and extracted solid tobacco material. The liquid extract may be at least partially separated from the solid tobacco material prior to the formation of the liquid composition. In some embodiments, the tobacco extract is used directly as or in the liquid composition.

[0067] The liquid tobacco extract may be an extract from any type of tobacco and any part of the tobacco plant, including tobacco lamina, stem, stalk, ribs, scraps and shorts 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 here. The tobacco may be expanded, such as dry-ice expanded tobacco (DIET), or processed by any other means. In some embodiments, the tobacco material may be reconstituted tobacco material. The tobacco may be pre-processed or unprocessed, and may be, for instance, solid stems (SS); shredded dried stems (SDS); steam treated stems (STS); or any combination thereof. The tobacco material may be fermented, cured, uncured, toasted, or otherwise pre-treated.

[0068] In some embodiments, the tobacco extract has a solids content of between about 40 and about 65 wt%, between about 45 and about 65 wt%, or between about 40 and about 60 wt% (calculated on a wet weight basis). In some embodiments, the water content of the tobacco extract is between about 35 wt% and about 65 wt%, or between about 35 and about 55 wt% (calculated on a wet weight basis). In some embodiments, the nicotine content of the tobacco extract is between about 1 wt% and about 5 wt% (calculated on a wet weight basis).

[0069] The liquid composition may be in the form of a slurry, a suspension, an emulsion or a solution. The liquid composition may comprise a botanical extract and a further solvent component. The solvent component may comprise water. Where other components are to be included in the dried material, these further components may be added separately or with the water. In some embodiments, the liquid composition may comprise from about 30 to about 70% v / v botanical extract, from about 40 to about 60% v / v botanical extract, or about 50% v / v botanical extract.

[0070] 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% on a wet weight basis. Additionally or alternatively, the water content of the liquid composition is up to about 95 wt%, up to about 90 wt%, up to about 85 wt%, up to about 80 wt%, up to about 75 wt%, 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% on a wet weight basis. In some embodiments, the water content of the liquid composition is from about 45 to about 90 wt %, or from about 55 to about 85 wt% on a wet weight basis.

[0071] The liquid composition may comprise 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% tobacco solids (calculated on a wet weight basis). Alternatively or additionally, the liquid composition may comprise 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% tobacco solids (calculated on a wet weight basis). In some embodiments, the liquid tobacco extract and / or the liquid composition comprises from about 10 wt% to about 65 wt% tobacco solids (calculated on a wet weight basis), or from about 25 wt% to about 45 wt%.

[0072] In some embodiments, the liquid composition comprises 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%, at least about 90 wt% tobacco extract (calculated on a wet weight basis). Alternatively or additionally, liquid composition comprises 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% tobacco extract (calculated on a wet weight basis). In some embodiments, the liquid composition comprises from about 40 to about 60 w% tobacco extract, or around 50 wt% tobacco extract (calculated on a wet weight basis).

[0073] In some embodiments, the liquid composition comprises an active substance. The active substance as used herein may be a physiologically active material, which is a material intended to achieve or enhance a physiological response.

[0074] In some embodiments, the active substance is derived from the botanical extract. For example, in some embodiments, the active substance is nicotine derived from the tobacco extract.

[0075] Alternatively or additionally, the liquid composition may comprise an active substance that is not derived from the botanical extract. Suitable active substances may be selected from nutraceuticals, nootropics and psychoactives. The active substance may be naturally occurring or synthetically obtained. The active substance may comprise for example, caffeine, taurine, theine, vitamins such as B6 or B12 or C, melatonin, cannabinoids, or constituents, derivatives, or combinations thereof. The active substance may comprise one or more constituents, derivatives or extracts of tobacco, cannabis or another botanical.

[0076] In some embodiments, the active substance may include nicotine derived from the tobacco extract and additional, added nicotine or other active substances mentioned herein. In some embodiments, the active substance comprises caffeine, melatonin or vitamin B12.

[0077] In some embodiments, the liquid composition comprises an extract from other botanical source(s) in addition to comprising a tobacco extract.

[0078] In some embodiments, the botanical extract is concentrated before it is included in the liquid composition. This may render the drying step more efficient, for example, requiring less energy. Also, this may help to provide the liquid composition in a form that is suitable for the process involving the formation of shaped portions of the liquid and their drying to form shaped particles.

[0079] In some embodiments, the liquid composition comprises one or more aerosol-former material. The aerosol-former material may comprise one or more constituents capable of forming an aerosol. The aerosol-former material may be, for instance, a polyol aerosol generator or a non-polyol aerosol generator. It may be a solid or liquid at room temperature, but preferably is a liquid at room temperature. In some embodiments, the aerosol-former material may comprise one or more of glycerine, glycerol, propylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, 1,3-butylene glycol, erythritol, meso-Erythritol, ethyl vanillate, ethyl laurate, a diethyl suberate, triethyl citrate, triacetin, a diacetin mixture, benzyl benzoate, benzyl phenyl acetate, tributyrin, lauryl acetate, lauric acid, myristic acid, and propylene carbonate.

[0080] In some embodiments, the aerosol-former material comprises one or more polyhydric alcohols, such as propylene glycol, triethylene glycol, 1,3-butanediol and glycerin; esters of polyhydric alcohols, such as glycerol mono-, di- or triacetate; and / or aliphatic esters of mono-, di- or polycarboxylic acids, such as dimethyl dodecanedioate and dimethyl tetradecanedioate. In some embodiments, the aerosol-former material comprises one or more compounds selected from erythritol, propylene glycol, glycerol, vegetable glycerine (VG), triacetin, sorbitol and xylitol. In some embodiments, the aerosol-former material comprises, consists essentially of, or consists of, glycerol. In a preferred embodiment, the aerosol-former material consists of glycerol.

[0081] A combination of aerosol-former materials may be used, in equal or differing proportions. The aerosol-former material may act as a plasticiser.

[0082] In some embodiments, the liquid composition comprises at least about 1% v / v, at least about 5% v / v, or at least about 10% v / v aerosol-former material. Alternatively or additionally, the liquid composition may comprise 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 aerosol-former material.

[0083] In embodiments of the invention in which the aerosol-forming material is glycerol, the dried shaped particles may comprise at least about 5 wt%, at least about 10 wt%, or at least about 12 wt% aerosol-former material (on a dry weight basis). Alternatively or additionally, the aerosol-forming material may comprise up to about 20 wt%, up to about 15 wt%, or up to about 20 wt% of glycerol (on a dry weight basis).

[0084] The amount of glycerol in the liquid composition, and therefore the dried shaped particles, is important because it acts as both an aerosol-former material and also a plasticizer. It is also important to remember that glycerol has anti-freeze properties. Whilst it is desirable to include sufficient glycerol to provide the consumer with an adequate and pleasing aerosol, a balance needs to be struck as the inclusion of too much glycerol will adversely affect the freeze-drying process. If the concentration of glycerol in the liquid composition is too high, this will lower the collapse temperature of the formulation, which means that freeze drying has to be carried out at a lower temperature, adding to the processing time required for drying and increasing the energy cost. If the collapse temperature of the formulation is low, the formulation will undergo structural changes. This may, for example, involve so-called "boiling" of the formulation, which will lead to a collapse of the product, with significant expansion of the dried particles being observed. Therefore, it is necessary for the freeze-drying to be conducted as a temperature below the collapse temperature of the formulation, and preferably from about 2 to 7°C below the collapse temperature.

[0085] In some embodiments, the amount of glycerol included in the liquid composition is no greater than 5 % v / v and it may be as low as 0%.

[0086] In some embodiments, the liquid composition further comprises one or more excipients.

[0087] The inventors have found that the inclusion of an excipient may be important for the stability of the liquid composition during the freeze-drying process, especially when the liquid composition comprises glycerol as an aerosol-former material. This may be as a result of the excipient increasing the collapse temperature of the formulation. Indeed, experiments have shown that drying of liquid compositions comprising a tobacco extract and glycerol but no excipient can result in the undesirable structural changes discussed above during freeze-drying. They observed some "puffing" or significant expansion of the droplets as they are dried, indicating a "boiling" of the liquid composition. In contrast, with the addition of an excipient such as dextran (for example, Dextran 70K), no such changes were observed when droplets were dried. Instead, uniform sized beads are formed showing slight shrinkage as compared to the size of the frozen droplets prior to freeze drying.

[0088] Suitable excipients include mannitol, sucrose, trehalose, lactose, sorbitol, raffinose, maltose, Dextran 10, Dextran 70, Dextran 90, maltodextrin, gelatin, agar, cyclodextrin, PEG 2000-6000, (PVP 10k).

[0089] In some embodiments, the liquid composition comprises one or more excipients in an amount of from about 1 to about 20 wt% on a wet weight basis. In some embodiments, the liquid composition may comprise 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% excipient on a wet weight basis. Alternatively or additionally, the liquid composition may comprise up to about 20 wt%, up to about 15 wt%, or up to about 10 wt% excipient on a wet weight basis.

[0090] In some embodiments, the liquid composition comprises about 50 wt% tobacco extract, from about 0 to about 10% v / v glycerol and about 10 wt% excipient. The tobacco extract may comprise from about 55 to about 62 wt% tobacco solids.

[0091] In some embodiments, the liquid composition may comprise an acid. The acid may be an organic acid. In some of these embodiments, the acid may be at least one of a monoprotic acid, a diprotic acid and a triprotic 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 alpha-hydroxy acid, carboxylic acid, dicarboxylic acid, tricarboxylic acid and keto acid. In some such embodiments, the acid may be an alpha-keto acid.

[0092] In some such embodiments, the acid may be at least one of succinic acid, lactic acid, benzoic acid, citric acid, tartaric acid, fumaric acid, levulinic acid, acetic acid, malic acid, formic acid, sorbic acid, benzoic acid, propanoic and pyruvic acid.

[0093] 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 of sulphuric acid, hydrochloric acid, boric acid and phosphoric acid.

[0094] In some embodiments, the preferred acid is lactic acid and / or levulinic acid.

[0095] The inclusion of an acid may be beneficial as presence of an acid may stabilise dissolved species in the tobacco extract. For example, the presence of the acid may reduce or substantially prevent evaporation of nicotine from the liquid composition before or during freezing and freeze drying, thereby reducing loss of nicotine during manufacturing.

[0096] In some embodiments, the liquid composition comprises one or more acid in an amount of from about 1 to about 5 wt% on a wet weight basis. In some embodiments, the liquid composition further comprises one or more flavours.

[0097] As used herein, the terms "flavour" and "flavourant" refer to materials which, where local regulations permit, may be used to create a desired taste, aroma or other somatosensorial sensation in a product for adult consumers. They may include naturally occurring flavour materials, botanicals, extracts of botanicals, synthetically obtained materials, or combinations thereof (e.g., tobacco, cannabis, licorice (liquorice), hydrangea, eugenol, Japanese white bark magnolia leaf, chamomile, fenugreek, clove, maple, matcha, menthol, Japanese mint, aniseed (anise), cinnamon, turmeric, Indian spices, Asian spices, herb, Wintergreen, cherry, berry, red berry, cranberry, peach, apple, orange, mango, clementine, lemon, lime, tropical fruit, papaya, rhubarb, grape, durian, dragon fruit, cucumber, blueberry, mulberry, citrus fruits, Drambuie, bourbon, scotch, whiskey, gin, tequila, rum, spearmint, peppermint, lavender, aloe vera, cardamom, celery, cascarilla, nutmeg, sandalwood, bergamot, geranium, khat, naswar, betel, shisha, pine, honey essence, rose oil, vanilla, lemon oil, orange oil, orange blossom, cherry blossom, cassia, caraway, cognac, jasmine, ylang-ylang, sage, fennel, wasabi, piment, ginger, coriander, coffee, hemp, a mint oil from any species of the genus Mentha, eucalyptus, star anise, cocoa, lemongrass, rooibos, flax, ginkgo biloba, hazel, hibiscus, laurel, mate, orange skin, rose, tea such as green tea or black tea, thyme, juniper, elderflower, basil, bay leaves, cumin, oregano, paprika, rosemary, saffron, lemon peel, mint, beefsteak plant, curcuma, cilantro, myrtle, cassis, valerian, pimento, mace, damien, marjoram, olive, lemon balm, lemon basil, chive, carvi, verbena, tarragon, limonene, thymol, camphene), flavour enhancers, bitterness receptor site blockers, sensorial receptor site activators or stimulators, sugars and / or sugar substitutes (e.g., sucralose, acesulfame potassium, aspartame, saccharine, cyclamates, lactose, sucrose, glucose, fructose, sorbitol, or mannitol), and other additives such as charcoal, chlorophyll, minerals, botanicals, or breath freshening agents. They may be imitation, synthetic or natural ingredients or blends thereof. They may be in any suitable form, for example, liquid such as an oil, solid such as a powder.

[0098] In some embodiments, the flavour comprises menthol, spearmint and / or peppermint. In some embodiments, the flavour comprises flavour components of cucumber, blueberry, citrus fruits and / or redberry. In some embodiments, the flavour comprises eugenol. In some embodiments, the flavour comprises flavour components extracted from tobacco. In some embodiments, the flavour comprises flavour components extracted from cannabis. In some embodiments, the flavour may comprise a sensate, which is intended to achieve a somatosensorial sensation which are usually chemically induced and perceived by the stimulation of the fifth cranial nerve (trigeminal nerve), in addition to or in place of aroma or taste nerves, and these may include agents providing heating, cooling, tingling, numbing effect. A suitable heat effect agent may be, but is not limited to, vanillyl ethyl ether and a suitable cooling agent may be, but not limited to eucolyptol, WS-3.

[0099] In some embodiments, the liquid composition comprises one or more flavours in an amount of from about 0.1 to about 5 wt%, or from about 1 to about 2 wt% on a wet weight basis.

[0100] Where a hydrophobic flavour is included in the liquid composition, it may be necessary to also include a surfactant or emulsifier to allow the formation of a stable oil-in-water emulsion. Suitable surfactants include, for example, those comprising fatty acid esters of polyoxyethylene sorbitan (Tweens) or sorbitan (Spans), or lecithins.

[0101] Manufacturing shaped particles in the form of beads

[0102] In order to form the shaped particles of the present invention in the form of beads, droplets of the liquid composition comprising a botanical extract are freeze dried. To enable the liquid to be freeze dried in the form of a droplet, the liquid composition is first dispensed as a series of droplets that are rapidly pre-frozen (also referred to herein as "snap frozen") by exposure to extreme cold.

[0103] In some embodiments, droplets of the liquid composition are dispensed into liquid nitrogen. The droplets of liquid composition will freeze very rapidly upon exposure to a temperature in the region of -196°C.

[0104] The size of the beads may be adjusted by adjusting the size of the droplets that are dispensed.

[0105] In some embodiments, droplets are formed with a volume of from about 1 to about 50 pl. In some embodiments, the volume of the droplets or the average (mean) volume is at least about 1 pl, at least about 5 pl, at least about 10 pl, at least about 15 pl, at least about 20 pl, at least about 25 pl, at least about 30 pl, at least about 35 pl or at least about 40 pl. Additionally or alternatively, in some embodiments, the volume of the droplets or the average (mean) volume is no greater than about 50 pl, about 45 pl, about 40 pl, about 35 pl, about 30 pl, about 25 pl, about 20 pl, or no greater than about 15 pl.

[0106] In some embodiments, the droplets are pre-frozen at atmospheric pressure.

[0107] The droplets of liquid composition tend to expand when pre-frozen. Their size may increase by from about 5 to about 10%. Some crystallisation may also be observed within the frozen droplets.

[0108] Once formed, the pre-frozen droplets of the liquid composition are freeze-dried.

[0109] Freeze

[0110] The shaped portions of the liquid composition are dried by freeze drying. In the embodiments mentioned above, the shaped portions may be spheroids, formed as frozen droplets.

[0111] In other embodiments, the shaped portions of the liquid composition may be created using a mould. In such embodiments, at least one surface of the shape created will be flat. The liquid composition may be added to the mould and then directly freeze- dried, with the mould being placed in the freeze drier. In other embodiments, the liquid in the mould may be frozen, for example by flash freezing, and the frozen portions may then be freeze-dried.

[0112] The drying methods used to dry the shaped portions of liquid composition may be any suitable freeze-drying process using known small or large scale freeze-drying equipment.

[0113] Freeze-drying, also known as lyophilisation or cryodesiccation, is a process in which the liquid composition is frozen, the temperature lowered and the water is removed via sublimation under reduced pressure conditions. Without wishing to be bound by any particular theory, it is believed that the low processing temperatures and rapid water loss via sublimation avoid changes in the liquid composition's structure, appearance and characteristics. This process preserves the structure of the liquid composition and reduces the loss and decomposition of volatile components, such as nicotine and flavour compounds.

[0114] Freeze drying may be conducted at a temperature of from about -35 to about -50°C. The freeze drying may be carried out at a pressure of from about 30 to about 40 pbar. The dried shaped particles formed by freeze drying have a lower water content than the shaped portion of liquid composition. The residual moisture content of the dried shaped particles may be reduced to less than about 15% and may be from about 5 to about 14% or from about 7 to about 12%, as measured by gas chromatographythermal conductivity detector (GC-TCD) or Karl Fischer measurement. A low moisture content helps to avoid or manage the phenomenon referred to as "hot puff" which may be seen in aerosol generating systems such as tobacco heating products.

[0115] The drying of the liquid composition to form the dried shaped particles may result in a reduction in 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%.

[0116] In some embodiments, the shaped portions of liquid composition are freeze-dried for a period of from 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.

[0117] In some embodiments, the freeze-dried shaped portions undergo a secondary drying step.

[0118] The first drying step, in which the liquid composition is dried by freeze drying, removes the unbound water in the liquid composition. The optional secondary drying step may be carried out to remove the chemically bound water and thereby further reduce the moisture content of the dried particles.

[0119] In some embodiments, the secondary drying step may comprise gradually increasing the temperature of the freeze-dried shaped particles to a temperature of from about + 15°C to about +25°C, for example, to a temperature of about +20°C and then holding the shaped particles at that temperature for a period of time. The temperature at which the freeze-dried shaped particles held during the secondary drying step must not be higher than room temperature, in order to avoid driving off desirable volatile components from the liquid composition that have been retained as a result of the pre-freezing and freeze-drying steps. In some embodiments, the endpoint of the secondary drying may be determined by vacuum gauge which is used to determine when no more water is being removed (i.e., the water release plateaus). In some embodiments, this may be when the moisture content is less than about 10%, as measured by Karl Fisher analysis.

[0120] In some embodiments, the shaped particles may be held at the elevated temperature for a period of from about 10 to about 25 hours.

[0121] Dried shaped particles

[0122] The shaped particles formed by drying shaped portions of a liquid composition comprising a botanical extract have a size, shape and make up that is readily controlled as a result of the manufacturing process discussed above.

[0123] The geometry of the shaped particles will be influenced by the geometry of the shaped portion of liquid composition that is dried. This in turn may be controlled by the method used to form the shaped portion, using, for example, pre-frozen droplets or moulds.

[0124] In addition, the freeze-drying process leads to some slight shrinkage of the shaped portion. The shrinkage observed occurs as a result of the removal of water from the frozen droplets and so the greater the water content in the liquid composition (and the frozen droplets), the greater the shrinkage that will be observed following drying. This shrinkage may result in a reduction in size or volume of from about 5 to 10%. The specific extent of the shrinkage will be dependent on the shape and size of the portion.

[0125] Where the shaped portion has been pre-frozen, this step may, as discussed above, result in an initial expansion. The subsequent shrinkage during freeze-drying may result in approximate return to the size before the pre-freezing.

[0126] In some embodiments, the shaped particles are beads that may be generally spheroid in shape. In some embodiments, the beads have the shape of a slightly shrunken sphere, i.e., they may have a slightly uneven surface morphology.

[0127] The diameter of the beads will be influenced by the volume of the droplet formed from the liquid composition and by the solids content in the liquid composition. Some shrinkage is observed during drying, relative to the size of the frozen droplets. The manufacturing process means that the size of the dried beads can be very consistent. In some embodiments, at least about 90% of the dried beads have a diameter that varies by no more than 5% from the mass median diameter of the population. 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 varies by no more than 5% from the mass median diameter of the population.

[0128] In some embodiments, the dried beads are free-flowing and non-sticky, and this aids handling of the beads.

[0129] In some embodiments, the dried beads have a diameter in the range of from about 2 mm to about 5 mm. Optionally, the diameter may 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 dried beads have a mean diameter of from about 2.5 to about 3 mm.

[0130] Beads with a smaller diameter have a greater surface area to volume ratio and they may therefore exhibit more rapid release of components compared to beads with a larger diameter.

[0131] In some embodiments, the size of the dried beads is selected to provide a desired release profile of one of more components. In general, beads with a smaller diameter or size will release components more quickly upon use and for a shorter period of time. Beads with a larger diameter or particle size will release components more gradually and for a longer period. In some embodiments, beads of different sizes may be selected and combined to provide a release profile that starts rapidly upon commencement of use and continues over an extended period of use.

[0132] In some embodiments, it may be desirable for the beads to have an average particle size or diameter of no greater than about 5 mm, of no greater than 4 mm, of no greater than about 3 mm, or of no greater than about 2 mm, when measured by sieving. In some embodiments, the beads have a diameter of from about 2 to about 3 mm. This may be assessed by sieving or by measurement using a QuickScope™ instrument for approximating the diameter of a roughly spherical form. In some embodiments, the dried beads have a volume in the range of from about 0.005 to about 0.02 cm3. In some embodiments, the dried beads have a mean volume of at least about 0.008 cm3, at least about 0.009 cm3, at least about 0.01 cm3, and / or a mean volume of no greater than about 0.015 cm3, no greater than about 0.014 cm3, no greater than about 0.013 cm3, or no greater than about 0.012 cm3.

[0133] In some embodiments, the dried shaped particles have a density in the range of from about 0.5 to about 1.5 g / cm3. In some embodiments, the shaped particles have a mean density of at least about 0.5 g / cm3, at least about 0.6 g / cm3, at least about 0.7 g / cm3, and / or a mean density of no greater than about 1.5 g / cm3, no greater than about 1.4 g / cm3, no greater than about 1.3 g / cm3, no greater than about 1.2 g / cm3, or no greater than about 1.1 g / cm3.

[0134] In some embodiments, the dried shaped particles have flat shapes, such as thin strips or discs. In some embodiments, the flat shapes have a thickness of from about 0.05 mm to about 1 mm. In some embodiments the thickness of the flat shapes 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 in addition, the thickness of the flat shapes is no more than about 1 mm, no more than about 0.9 mm, no more than about 0.8 mm, no more than about 0.7 mm, no more than about 0.6 mm, no more than about 0.5 mm, no more than about 0.45 mm, no more than about 0.4 mm, no more than about 0.35 mm, no more than about 0.3 mm, no more than about 0.25 mm, no more than about 0.2 mm, no more than about 0.15 mm, no more than about 0.1 mm, no more than about 0.09 mm, no more than about 0.08 mm, no more than about 0.07 mm, or no more than about 0.06 mm.

[0135] In some embodiments, the flat shape matches that of cut rag tobacco, for example having a width of from about 0.8 to about 1.2 mm, a length of from about 10 to about 40 mm, and a thickness of from about 0.06 to about 0.2 mm.

[0136] The chemical makeup of the dried shaped particles will be controlled by the chemical makeup of the liquid composition. The drying process is selected to mitigate or prevent the loss of desirable components from the liquid composition, including in particular the loss of components of the botanical extract. Where the botanical extract is a tobacco extract, it is desirable to retain tobacco components such as nicotine and volatile or semi-volatile flavours and aromas. In some embodiments, the drying process removes essentially only water from the liquid composition. In other embodiments, some nicotine and / or glycerol is also lost during the drying process, as both are soluble in water.

[0137] In some embodiments, the dried shaped particles comprise dried botanical extract, for example, dried tobacco extract. Optionally, the shaped particles may further comprise an aerosol-former material. In some embodiments, the shaped particles also comprise an excipient.

[0138] In some embodiments, the dried shaped particles comprise from about 45 to about 100% by weight dried tobacco extract. For example, the shaped particles 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%, at least about 90 wt% tobacco extract (calculated on a dry weight basis). Alternatively or additionally, dried particles 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% tobacco extract (calculated on a dry weight basis). In some embodiments, the dried particles comprise from about 55 to about 85 wt% or from about 50 to about 80 wt% dried tobacco extract (calculated on a dry weight basis).

[0139] In some embodiments, the amount of tobacco extract included in the dried shaped particles is as high as possible to provide as much nicotine and tobacco-derived flavours and aromas as possible per unit weight of material. This high concentration of the tobacco components will have an impact on the weight and volume of material that needs to be shipped, stored and incorporated into an eventual final product.

[0140] In some embodiments, the dried shaped particles may comprise about 3-6 wt% of nicotine (calculated on a dry weight basis) derived from the tobacco extract. If additional nicotine is added, the total nicotine content of the particles may be increased, for example up to about 10 wt%.

[0141] In some embodiments, the dried shaped particles have a residual moisture content of greater than 7% and no more than 12%, or not more than 10%.

[0142] The water content of the shaped particles described herein may vary according to, for example, the temperature, pressure and humidity conditions at which the particles are maintained. The water content can be determined by Karl-Fisher analysis or by gas chromatography-thermal conductivity detector (GC-TCD), as known to those skilled in the art.

[0143] After manufacture of the dried shaped particles, it may be desirable to store the particles in a controlled, dry environment, to reduce the likelihood of the particles absorbing moisture from their immediate environment. Ideally, the dried particles will be protected from moisture until they are to be used by a consumer.

[0144] In some embodiments, the dried shaped particles comprise from about 0.1 to about 30% by weight aerosol-former material. In some embodiments, the amount of aerosol-former material in the dried particles is from about 1 to about 25% by weight (dry weight basis), from about 5 to about 20% or from about 5 to about 15%.

[0145] The aerosol-former may be included in dried shaped particles that are intended for use as an aerosol-generating material. Upon heating the dried particles comprising an aerosol-former material, a vapour and / or aerosol may be formed with desirable properties. In addition, the aerosol-former material may promote and control the release of the botanical components from the dried particles.

[0146] Aerosol-former materials, such as glycerol and others mentioned herein, are humectants and therefor can encourage the dried shaped particles to hold and absorb moisture. Higher moisture content of the dried particles can lead to the particles becoming tacky or sticky and becoming more difficult to handle. The performance of the dried particles in delivering components can be compromised by the additional moisture content and the inferior handleability. Also, it is wasteful for time and energy to be expended drying the shaped particles, only for them to absorb moisture before they are used.

[0147] In addition, as discussed above and in the examples, the amount of aerosol-former material has also been found to affect the results of the drying process and the optimal freeze-drying conditions. Where greater amounts of aerosol-former material are included in the liquid composition, fragmentation of the dried particles was more frequently observed, providing particles of unpredictable size and shape.

[0148] Finally, at least some of the aerosol-former materials proposed for inclusion in the shaped particles, such as glycerol, also act an anti-freeze agent. As a result, these materials will affect how the liquid composition acts when exposed to the freezing temperatures during the pre-freezing and freeze-drying steps. Therefore, an 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.

[0149] In some embodiments, the dried shaped particles comprise from about 0.1 to about 25% by weight excipient. In some embodiments, the amount of excipient in the dried particles is from about 5 to about 20% by weight (dry weight basis).

[0150] The excipient is included in the dried shaped particles to stabilise the liquid composition as it is frozen and dried. As discussed in the examples, the presence and the amount of excipient has been found to affect the results of the drying process.

[0151] The liquid composition needs to be freeze-dried below the collapse temperature. The presence of an excipient can increase the collapse temperature of the liquid composition, thereby allowing freeze-drying at a higher temperature without increasing the risk of product collapse, which can result in "puffing", with large, expanded particles being produced with very different properties to the unpuffed particles, resulting in a significantly inferior product.

[0152] The dried shaped particles disclosed herein may be used in a variety of different delivery systems, in order to deliver components of the tobacco extract to a user.

[0153] As used herein, the term "delivery system" is intended to encompass systems that deliver at least one substance to a user, and includes: combustible aerosol provision systems, such as cigarettes, cigarillos, cigars, and tobacco for pipes or for roll-your-own or for make-your-own cigarettes (whether based on tobacco, tobacco derivatives, expanded tobacco, reconstituted tobacco, tobacco substitutes or other smokable material); non-combustible aerosol provision systems that release compounds from an aerosol-generating material without combusting the aerosol-generating material, such as electronic cigarettes, tobacco heating products, and hybrid systems to generate aerosol using a combination of aerosol-generating materials; and aerosol-free delivery systems that deliver the at least one substance to a user orally, nasally, transdermally or in another way without forming an aerosol, including but not limited to, lozenges, gums, patches, articles comprising inhalable powders, and oral products such as oral tobacco which includes snus or moist snuff, wherein the at least one substance may or may not comprise nicotine. In some embodiments, the dried shape particles are used in a delivery system without significant further processing. For example, the particle size may not need to be adjusted or selected.

[0154] Aerosol generating material

[0155] The dried shaped particles of the present invention may be used as an aerosolgenerating material. An aerosol-generating material is a material that is capable of generating aerosol, for example when heated, irradiated or energized in any other way.

[0156] In some embodiments, the aerosol-generating material is for use in a "noncombustible" aerosol provision system. According to the present disclosure, a "non-combustible" aerosol provision system is one where a constituent aerosolgenerating material of the aerosol provision system (or component thereof) is not combusted or burned in order to facilitate delivery of at least one substance to a user.

[0157] In some embodiments, the delivery system is a non-combustible aerosol provision system, such as a powered non-combustible aerosol provision system.

[0158] In some embodiments, the non-combustible aerosol provision system is an electronic cigarette, also known as a vaping device or electronic nicotine delivery system (END), although it is noted that the presence of nicotine in the aerosolgenerating material is not a requirement.

[0159] In some embodiments, the non-combustible aerosol provision system is an aerosol-generating material heating system, also known as a heat-not-burn system. An example of such a system is a tobacco heating system.

[0160] In some embodiments, the non-combustible aerosol provision system is a hybrid system to generate aerosol using a combination of aerosol-generating materials, one or a plurality of which may be heated. Each of the aerosol-generating materials may be, for example, in the form of a solid, liquid or gel and may or may not contain nicotine. In some embodiments, the hybrid system comprises a liquid or gel aerosol-generating material and a solid aerosol-generating material. The solid aerosol-generating material may comprise, for example, tobacco or a non-tobacco product. Typically, the non-combustible aerosol provision system may comprise a noncombustible aerosol provision device and a consumable for use with the noncombustible aerosol provision device.

[0161] In some embodiments, the disclosure relates to consumables comprising aerosolgenerating material and configured to be used with non-combustible aerosol provision devices. These consumables are sometimes referred to as articles throughout the disclosure.

[0162] In some embodiments, the non-combustible aerosol provision system, such as a non-combustible aerosol provision device thereof, may comprise a power source and a controller. The power source may, for example, be an electric power source or an exothermic power source. In some embodiments, the exothermic power source comprises a carbon substrate which may be energised so as to distribute power in the form of heat to an aerosol-generating material or to a heat transfer material in proximity to the exothermic power source.

[0163] In some embodiments, the non-combustible aerosol provision system may comprise an area for receiving the consumable, an aerosol generator, an aerosol generation area, a housing, a mouthpiece, a filter and / or an aerosol-modifying agent.

[0164] In some embodiments, the consumable for use with the non-combustible aerosol provision device may comprise aerosol-generating material, an aerosol-generating material storage area, an aerosol-generating material transfer component, an aerosol generator, an aerosol generation area, a housing, a wrapper, a filter, a mouthpiece, and / or an aerosol-modifying agent.

[0165] The dried shaped particles of the present disclosure provide aerosol-generating material that is stable at a range of temperatures, so that it may be stored and / or transported for a much longer period without deterioration of the properties of the aerosol. A low water content also inhibits microbial growth.

[0166] In some embodiments, a consumable comprises from about 50 to about 250 mg of the shaped particles, from about 50 to about 200 mg, from about 50 to about 150 mg, or about 100 mg of the shaped particles. In some embodiments, the dried shaped particles are the only aerosol-generating material used, or they are the only solid aerosol-generating material used to generate an aerosol.

[0167] In other embodiments, the dried shaped particles of the present invention may be combined with one or more other aerosol-generating materials. For example, the dried shaped particles may be combined with aerosol-generating material comprising tobacco material, or other plant or botanical material. The different aerosolgenerating materials may be provided separately or together, for example as a mixture or blend.

[0168] In some embodiments, the aerosol-generating material comprises one or more cannabinoid compounds selected from the group consisting of: cannabidiol (CBD), tetrahydrocannabinol (THC), tetrahydrocannabinolic acid (THCA), cannabidiolic acid (CBDA), cannabinol (CBN), cannabigerol (CBG), cannabichromene (CBC), cannabicyclol (CBL), cannabivarin (CBV), tetrahydrocannabivarin (THCV), cannabidivarin (CBDV), cannabichromevarin (CBCV), cannabigerovarin (CBGV), cannabigerol monomethyl ether (CBGM) and cannabielsoin (CBE), cannabicitran (CBT).

[0169] The aerosol-generating material may comprise one or more cannabinoid compounds selected from the group consisting of cannabidiol (CBD) and THC (tetrahydrocannabinol).

[0170] The aerosol-generating material may comprise cannabidiol (CBD).

[0171] The aerosol-generating material may comprise nicotine and cannabidiol (CBD).

[0172] The aerosol-generating material may comprise nicotine, cannabidiol (CBD), and THC (tetrahydrocannabinol).

[0173] Incorporation into an aerosol-generating device.

[0174] In some embodiments, the dried shaped particles are provided in a consumable.

[0175] A consumable is an article comprising aerosol-generating material, part or all of which is intended to be consumed during use by a user. A consumable may comprise one or more other components, such as an aerosol-generating material storage area, an aerosol-generating material transfer component, an aerosol generation area, a housing, a wrapper, a mouthpiece, a filter and / or an aerosol-modifying agent. A consumable may also comprise an aerosol generator, such as a heater, that emits heat to cause the aerosol-generating material to generate aerosol in use. The heater may, for example, comprise combustible material, a material heatable by electrical conduction, or a susceptor. The consumable may be any shape or size that is appropriate to the aerosol provision device. In some embodiments, the consumable is a rod shape.

[0176] In some embodiments, a population of dried shaped particles is provided in an aerosol-generating device such as a tobacco-heating product (THP) or hybrid e- cigarette product. Advantageously, the dried shaped particles may be used directly as a solid substrate and are directly heated without burning to provide an inhalable aerosol. Heating the particles may aerosolise components of the dried particles, for example the glycerol, nicotine and / or tobacco flavour. The dried shaped particles and / or the consumable may be stored in reduced humidity conditions, for example less than about 30% humidity, prior to use.

[0177] An additional benefit of the dried shaped particles being used directly as a solid substrate is that the low water content reduces issues associated with "hot puff", which are known in the art.

[0178] Figure 1 is a side-on cross-sectional view of a consumable or article 1 for use in an aerosol delivery system. The article 1 comprises a mouthpiece segment 2, and an aerosol generating segment 3.

[0179] The aerosol generating segment 3 is in the form of a cylindrical rod and comprises an aerosol-generating material 4 comprising a population of dried shaped particles as disclosed herein. For example, the dried shaped particles can be any of the particles or beads discussed herein.

[0180] Although described above in rod form, the aerosol-generating segment 3 can be provided in other forms, for instance a plug, pouch, or packet of material within an article.

[0181] The mouthpiece segment 2, in the illustrated embodiment, includes a body of material 5 such as a fibrous or filamentary tow. The rod-shaped consumable 1 further comprises a wrapper 6 circumscribing the mouthpiece segment 2 and aerosol generating segment 3, such as a paper wrapper.

[0182] Figure 2 shows an example of a non-combustible aerosol provision device 100 for generating aerosol from an aerosol-generating medium such as the aerosol-generating material of a consumable 110, as described herein. In broad outline, the device 100 may be used to heat a replaceable article 110 comprising the aerosol-generating medium, for instance an article 1 as illustrated in Figure 1 or as described elsewhere herein, to generate an aerosol or other inhalable medium which is inhaled by a user of the device 100. The device 100 and replaceable article 110 together form a system.

[0183] The device 100 comprises a housing 102 (in the form of an outer cover) which surrounds and houses various components of the device 100. The device 100 has an opening 104 in one end, through which the article 110 may be inserted for heating by a heating assembly. In use, the article 110 may be fully or partially inserted into the heating assembly where it may be heated by one or more components of the heater assembly.

[0184] The device 100 of this example comprises a first end member 106 which comprises a lid 108 which is moveable relative to the first end member 106 to close the opening 104 when no article 110 is in place. In Figure 2, the lid 108 is shown in an open configuration, however the lid 108 may move into a closed configuration. For example, a user may cause the lid 108 to slide in the direction of arrow "B".

[0185] 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 may turn on the device 100 by operating the switch 112.

[0186] The device 100 may also comprise an electrical component, such as a socket / port 114, which can receive a cable to charge a battery of the device 100. For example, the socket 114 may be a charging port, such as a USB charging port.

[0187] Aerosol free delivery

[0188] In some embodiments, the delivery system is an aerosol-free delivery system that delivers at least one substance to a user orally, nasally, transdermally or in another way without forming an aerosol, including but not limited to, lozenges, gums, patches, articles comprising inhalable powders, and oral products such as oral tobacco which includes snus or moist snuff, wherein the at least one substance may or may not comprise nicotine.

[0189] In some embodiments, the dried shaped particles are incorporated into a pouch for oral use. The dried shaped particles may be the only material included in the pouch or they may be combined with other materials including other sources of active and / or flavour substances.

[0190] One example of a permeable pouch is shown in Figure 3. The pouch 21 comprises two sheets 22 of porous material. These sheets are fused or adhered along their edges to form a chamber within which a flavour- and / or active-delivering composition 23 is sealed. This flavour- and / or active-delivering composition comprises dried shaped particles as disclosed herein.

[0191] Because the dried shaped particles provide the botanical, for example tobacco, extract in a highly concentrated form, an oral pouch may be very small whilst still providing the physiological and organoleptic impact of a much larger, conventional oral pouch. This may have benefits for the user in terms of comfort during use, or discreteness of the product.

[0192] In some embodiments, the use of a polysaccharide such as dextran as an excipient means that the dried shaped particles may have a sweet taste when placed in the mouth. This may reduce the need to include further or any additional sweetener or flavour.

[0193] Other possible aerosol-free delivery systems that include the dried shaped particles disclosed herein deliver components to a user orally, nasally, transdermally or by any other suitable route of administration. In some embodiments, the shaped particles are incorporated into a product selected from the group consisting of: lozenges, gums, patches, and inhalable powders.

[0194] Examples

[0195] Example 1 - Nicotine retention

[0196] The nicotine content of the liquid composition and dried beads after the freeze-drying process has been calculated, providing an indication of the amount of nicotine retained following the processing. Compared to the original tobacco extract, the nicotine recovery of the dried aerosol generating material is at least about 50 wt% on a dry weight basis. The nicotine recovery of the dried aerosol generating material compared to the original tobacco extract may be at least about 55%, at least about 60%, at least about 75%, at least about 80%, or at least about 90% on a dry weight basis.

[0197] Example 2 - Glycerol retention

[0198] The glycerol content of the precursor and dried aerosol-generating material after the freeze-drying process has been calculated, providing an indication of the amount of glycerol retained following the processing. Compared to the precursor material, the glycerol recovery of the dried aerosol generating material is at least about 50%. The glycerol recovery of the dried aerosol generating material compared to the precursor material may 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% at least about 95% on a dry weight basis.

[0199] Example 3

[0200] 1. Liquid compositions

[0201] A series of liquid composition samples were prepared according to the makeup set out in Table 1 below.

[0202] The liquid aqueous tobacco extracts were combined with an equal volume of solvent comprising an aqueous solution of excipient and / or aerosol former material. The excipient used was Dextran 70. The aerosol-former material used was glycerol. Three different aqueous tobacco extracts were used to see the impact of this component on the process and product.

[0203] Table 1

[0204] 2. Snap-freezing droplets Droplets with a volume of approximately 20 pl were dispensed in a vacuum flask (Dewar flask) containing liquid nitrogen. The frozen droplets formed from each of the samples were then transferred into a separate vial at a temperature of -50°C and atmospheric pressure. The frozen droplets were uniform in size and shape, although there was some variation in colour. The frozen droplets were substantially spherical.

[0205] 3. Primary (freeze) drying stage

[0206] The frozen droplets were freeze dried at a temperature of -50°C and a pressure of 30 pbar for a period of 5380 minutes.

[0207] 4. Secondary drying stage

[0208] The temperature of the freeze-dried beads was then adjusted to 20°C over a period of 140 minutes. The pressure was maintained at 30 pbar. Once at the target temperature of 20°C, the beads were held at this temperature and at a pressure of 30 pbar for a further period of 1250 minutes.

[0209] The properties of the resultant dried beads are summarised in Table 2.

[0210] Table 2

[0211] From the comments set out above, the following conclusions could be drawn.

[0212] The excipient Dextran 70 was found to stabilise the liquid composition during the drying process and appeared to prevent the undesirable puffing (expansion) that was observed. Not all beads in the batch suffered from this phenomenon, but a proportion of the dried material was not suitable for use as a result when no excipient was included in the liquid composition. The absence of an excipient also resulted in incomplete drying in sample no. 1.

[0213] The amount of glycerol included appeared to have a small impact on the product's appearance and did not seem to adversely affect the drying process at -50°C, despite the anti-freeze properties.

[0214] Example 4

[0215] The effect of the inclusion of glycerol and excipient (in this case Dextran 70) on the collapse temperature of formulations was assessed with the results shown in Table 3.

[0216] Table 3

[0217] As can be seen from this data, the inclusion of glycerol decreased the collapse temperature. This means that formulations that comprise glycerol need to be freeze- dried at lower temperatures (and for longer periods).

[0218] The data also indicates that the inclusion of dextran as an excipient increased the collapse temperature. This means that some of the effect of including glycerol in the liquid composition may be compensated for by including an excipient. Also, the inclusion of the excipient makes the freeze-drying process cheaper and faster, as it increases the temperature at which the process may be carried out without risking collapse of the formulation and the unacceptable effect of that collapse on the resultant dried composition.

[0219] The various embodiments described herein are presented only to assist in understanding and teaching the claimed features. These embodiments are provided as a representative sample of embodiments only, and are not exhaustive and / or exclusive. It is to be understood that advantages, embodiments, examples, functions, features, structures, and / or other aspects described herein are not to be considered limitations on the scope of the invention as defined by the claims or limitations on equivalents to the claims, and that other embodiments may be utilised and modifications may be made without departing from the scope of the claimed invention. Various embodiments of the invention may suitably comprise, consist of, or consist essentially of, appropriate combinations of the disclosed elements, components, features, parts, steps, means, etc., other than those specifically described herein. In addition, this disclosure may include other inventions not presently claimed, but which may be claimed in future.

Claims

Claims1. Shaped particles each comprising a freeze-dried shaped portion of a liquid composition comprising a botanical extract.

2. Shaped particles as claimed in claim 1, wherein the shaped particles comprise volatile and semi-volatile components of the botanical extract.

3. Shaped particles as claimed in claim 1 or claim 2, wherein the botanical extract is a tobacco extract, and optionally an aqueous tobacco extract.

4. Shaped particles as claimed in any one of claims 1 to 3, the liquid composition further comprising an aerosol-former material.

5. Shaped particles as claimed in claim 4, wherein the aerosol-former material is glycerol.

6. Shaped particles as claimed in any one of claims 1 to 5, the liquid composition further comprising an excipient.

7. Shaped particles as claimed in any one of claims 1 to 6, wherein the excipient is a dextran.

8. Shaped particles as claimed in any one of claims 1 to 7, comprising from about 45 to about 100% by weight dried botanical extract (on a dry weight basis).

9. Shaped particles as claimed in any one of claims 1 to 8, comprising from about 1 to about 20% by weight aerosol-former material (on a dry weight basis).

10. Shaped particles as claimed in any one of claims 1 to 9, comprising from about 0.1 to about 20% by weight of an excipient (on a dry weight basis).

11. Shaped particles as claimed in any one of claims 1 to 10, wherein the shaped particles are freeze-dried droplets of the liquid composition comprising a botanical extract.

12. Shaped particles as claimed in any one of claims 1 to 11, wherein the shaped particles are spheroid beads.

13. Shaped particles as claimed in claim 12, wherein at least 90% of the beads have a diameter that varies by no more than 5% from the mass median diameter of the population.

14. Shaped particles as claimed in claim 12 or claim 13, wherein the beads have a diameter in the range of from about 2 mm to about 5 mm.

15. Shaped particles as claimed in any one of claims 12 to 14, wherein the beads have a volume of from about 0.005 to about 0.02 cm3.

16. Shaped particles as claimed in any one of claims 1 to 15, wherein the shaped particles have a density in the range of from about 0.5 to about 1.5 g / cm3.

17. Shaped particles as claimed in any one of claims 1 to 11, wherein shaped particles are flat shapes, such as thin strips or discs.

18. Shaped particles as claimed in claim 17, having a thickness of from about 0.05 mm to about 1 mm.

19. Shaped particles as claimed in 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 Fisher analysis.

20. Shaped particles as claimed in claim 19, having a residual moisture content of at least 7%, as measured by Karl Fisher analysis.

21. A method of providing shaped particles, comprising : providing portions of a liquid composition comprising a botanical 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 comprising a botanical extract; and freeze-drying the frozen droplets to form beads.

23. A method as claimed in claim 22, wherein the droplets of the liquid composition comprising a botanical extract have a volume of from about 1 pl to about 50 pl.

24. A method as claimed in claim 22 or claim 23, wherein the droplets are prefrozen by dispensing droplets of the liquid composition into liquid nitrogen.

25. A method as claimed in claim 24, wherein the droplets are pre-frozen at atmospheric pressure.

26. A method as claimed in claim 24 or claim 25, wherein the droplets are frozen instantaneously on contact with the liquid nitrogen.

27. A method as claimed in any one of claims 21 to 26, wherein the freeze-drying is carried out at a temperature of from about -35 to about -50°C28. A method as claimed in any one of claims 21 to 27, wherein the freeze-drying is carried out at a pressure of from about 30 to about 40 pbar.

29. A method as claimed in any one of claims 21 to 28, wherein the freeze-drying is carried out for a period of from about 48 hours to about 120 hours.

30. A method as claimed in any one of claims 21 to 29, comprising a secondary drying step.

31. A method as claimed in claim 30, wherein the secondary drying step involves increasing the temperature of the freeze-dried shaped particles to a secondary drying temperature of no more than 20°C.

32. A method as claimed in 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. A method as claimed in any one of claims 30 to 32, wherein the secondary drying step is carried out at a pressure of from about 20 to about 30 pbar.

34. A non-combustible aerosol-provision system comprising shaped particles as claimed in any one of claims 1 to 20.

35. A non-combustible aerosol-provision system as claimed in 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 as claimed in claim 34 or claim 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 shaped particles as claimed in any one of claims 1 to 20.

38. An oral product comprising a permeable container surrounding shaped particles as claimed in any one of claims 1 to 20.

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

40. Use of a shaped particle as claimed in any one of claims 1 to 20 to generate an inhalable medium.

41. A shaped particle obtained or obtainable by a method as claimed in any one of claims 21 to 33, for use in an aerosol provision system to generate an inhalable medium.

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