Pouch products with improved flavor stability
By adding organic acids and microcrystalline cellulose derivatives to tobacco products to control pH values, the color changes and instability of the products are solved, and better stability and user experience are achieved.
Patent Information
- Application Number
- JP2022515865
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2019-09-11
- Filing Date
- 2020-09-10
- Publication Date
- 2025-04-16
- Estimated Expiration
- 2040-09-10
AI Technical Summary
Existing tobacco products are prone to color changes and instability during storage and use, resulting in a decline in product quality and poor user experience.
By adding one or more organic acids, such as citric acid, oxalic acid, acetic acid, etc. to the product, combining microcrystalline cellulose and its derivatives as filler materials, and controlling the pH value of the product between 5.5 and 6.5, a stable mixture is formed.
It significantly improves the color stability and taste durability of the product, extends the service life of the product, and improves the user's experience.
Smart Images

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Abstract
Description
[Technical field]
[0001] The present disclosure relates to flavored products intended for human consumption. The products are configured for oral use and deliver substances such as flavors and / or active ingredients during use. Such products may contain tobacco or tobacco-derived products or may be tobacco-free alternatives. [Background technology]
[0002] Tobacco can be enjoyed in so-called "smokeless" forms. Particularly well-known smokeless tobacco products are used by inserting some form of processed tobacco or tobacco-containing formulation into the mouth of the user. Traditional formats for such smokeless tobacco products include moist snuff, snus, and chewing tobacco, which are typically formed almost entirely from granular, granular, or shredded tobacco and are either divided by the user or presented to the user in individual portions such as single-use pouches or sachets. Other traditional forms of smokeless products include compressed or agglomerated forms such as wads, tablets, pellets, etc. Alternative product forms are also known, such as tobacco-containing gums and mixtures of tobacco with other plant materials.See, for example, U.S. Pat. No. 1,376,586 to Schwartz, U.S. Pat. No. 4,513,756 to Pittman et al., U.S. Pat. No. 4,528,993 to Sensabaugh Jr. et al., U.S. Pat. No. 4,624,269 to Story et al., U.S. Pat. No. 4,991,599 to Tibbetts, U.S. Pat. No. 4,987,907 to Townsend, U.S. Pat. No. 5,092,352 to Sprinkle, III et al., U.S. Pat. No. 5,387,416 to White et al., U.S. Pat. No. 6,668,839 to Williams, and U.S. Pat. No. 6,820,626 to Williams. No. 34,654 to Atchley et al., U.S. Pat. No. 6,953,040 to Atchley et al., U.S. Pat. No. 7,032,601 to Atchley et al., and U.S. Pat. No. 7,694,686 to Atchley et al., U.S. Pat. Application Publication No. 2004 / 0020503 to Williams, U.S. Pat. Application Publication No. 2005 / 0115580 to Quinter et al., U.S. Pat. Application Publication No. 2006 / 0191548 to Strickland et al., U.S. Pat. Application Publication No. 2007 / 0062549 to Holton Jr. et al., U.S. Pat. See the types, ingredients, and processing methods of smokeless tobacco formulations set forth in U.S. Patent Application Publication No. 2007 / 0186941 to Jr. et al., U.S. Patent Application Publication No. 2007 / 0186942 to Strickland et al., U.S. Patent Application Publication No. 2008 / 0029110 to Dube et al., U.S. Patent Application Publication No. 2008 / 0029116 to Robinson et al., U.S. Patent Application Publication No. 2008 / 0173317 to Robinson et al., U.S. Patent Application Publication No. 2008 / 0209586 to Neilsen et al., U.S. Patent Application Publication No. 2009 / 0065013 to Essen et al., and U.S. Patent Application Publication No. 2010 / 0282267 to Atchley, and WO 2004 / 095959 to Arnarp et al., each of which is incorporated herein by reference.
[0003] Smokeless tobacco product configurations that combine tobacco materials with a variety of binders and fillers have been proposed more recently, with exemplary product formats including lozenges, pastilles, gels, extruded forms, and the like. See, for example, U.S. Patent Application Publication No. 2008 / 0196730 to Engstrom et al., U.S. Patent Application Publication No. 2008 / 0305216 to Crawford et al., U.S. Patent Application Publication No. 2009 / 0293889 to Kumar et al., U.S. Patent Application Publication No. 2010 / 0291245 to Gao et al., U.S. Patent Application Publication No. 2011 / 0139164 to Mua et al., U.S. Patent Application Publication No. 2012 / 0037175 to Cantrell et al., U.S. Patent Application Publication No. 2012 / 0055494 to Hunt et al., U.S. Patent Application Publication No. 2012 / 0138073 to Cantrell et al., U.S. Patent Application Publication No. 2012 / 0138074 to Cantrell et al., U.S. Patent Application Publication No. 2013 / 0074855 to Holton Jr., and U.S. Patent Application Publication No. 2014 / 007616 to Holton Jr. See the types of products described in U.S. Patent Application Publication No. 2013 / 0074856 to Jr., U.S. Patent Application Publication No. 2013 / 0152953 to Mua et al., U.S. Patent Application Publication No. 2013 / 0274296 to Jackson et al., U.S. Patent Application Publication No. 2015 / 0068545 to Moldoveanu et al., U.S. Patent Application Publication No. 2015 / 0101627 to Marshall et al., and U.S. Patent Application Publication No. 2015 / 0230515 to Lampe et al., each of which is incorporated herein by reference.
[0004] All-white snus portions are growing in popularity, offering a distinct and aesthetically pleasing alternative to traditional snus. Such modern "white" pouch products may contain bleached tobacco or may be tobacco-free. Products of this type may suffer from certain drawbacks, such as reduced product stability, which may lead to product discoloration and / or undesirable organoleptic properties. It would therefore be desirable in the art to provide a product configured for oral use with increased stability to provide a more enjoyable user experience. [Prior art documents] [Patent documents]
[0005] [Patent Document 1] U.S. Pat. No. 1,376,586 [Patent Document 2] U.S. Pat. No. 4,513,756 [Patent Document 3] U.S. Pat. No. 4,528,993 [Patent Document 4] U.S. Pat. No. 4,624,269 [Patent Document 5] U.S. Pat. No. 4,991,599 [Patent Document 6] U.S. Pat. No. 4,987,907 [Patent Document 7] U.S. Patent No. 5,092,352 [Patent Document 8] U.S. Pat. No. 5,387,416 [Patent Document 9] U.S. Patent No. 6,668,839 [Patent Document 10] U.S. Patent No. 6,834,654 [Patent Document 11] U.S. Patent No. 6,953,040 [Patent Document 12] U.S. Patent No. 7,032,601 [Patent Document 13] U.S. Patent No. 7,694,686 [Patent Document 14] US Patent Application Publication No. 2004 / 0020503 [Patent Document 15] US Patent Application Publication No. 2005 / 0115580 [Patent Document 16] US Patent Application Publication No. 2006 / 0191548 [Patent Document 17] US Patent Application Publication No. 2007 / 0062549 [Patent Document 18] US Patent Application Publication No. 2007 / 0186941 [Patent Document 19] US Patent Application Publication No. 2007 / 0186942 [Patent Document 20] US Patent Application Publication No. 2008 / 0029110 [Patent Document 21] US Patent Application Publication No. 2008 / 0029116 [Patent Document 22] US Patent Application Publication No. 2008 / 0173317 [Patent Document 23] US Patent Application Publication No. 2008 / 0209586 [Patent Document 24] US Patent Application Publication No. 2009 / 0065013 [Patent Document 25] US Patent Application Publication No. 2010 / 0282267 [Patent Document 26] International Publication No. 2004 / 095959 [Patent Document 27] US Patent Application Publication No. 2008 / 0196730 [Patent Document 28] US Patent Application Publication No. 2008 / 0305216 [Patent Document 29] US Patent Application Publication No. 2009 / 0293889 [Patent Document 30] US Patent Application Publication No. 2010 / 0291245 [Patent Document 31] US Patent Application Publication No. 2011 / 0139164 [Patent Document 32] US Patent Application Publication No. 2012 / 0037175 [Patent Document 33] US Patent Application Publication No. 2012 / 0055494 [Patent Document 34] US Patent Application Publication No. 2012 / 0138073 [Patent Document 35] US Patent Application Publication No. 2012 / 0138074 [Patent Document 36] US Patent Application Publication No. 2013 / 0074855 [Patent Document 37] US Patent Application Publication No. 2013 / 0074856 [Patent Document 38] US Patent Application Publication No. 2013 / 0152953 [Patent Document 39] US Patent Application Publication No. 2013 / 0274296 [Patent Document 40] US Patent Application Publication No. 2015 / 0068545 [Patent Document 41] US Patent Application Publication No. 2015 / 0101627 [Patent Document 42] US Patent Application Publication No. 2015 / 0230515 Summary of the Invention
[0006] The present disclosure generally provides a product configured for oral use, and further provides a method for stabilizing flavor components present in the product. The product is intended to impart taste when used orally, and typically also provides an active ingredient, such as nicotine, to the consumer. The product and method rely on the surprising discovery that adding one or more organic acids to a mixture comprising one or more particulate filler components, water, and one or more flavoring agents results in a product that exhibits enhanced flavor stability compared to a product that does not include one or more organic acids.
[0007] Thus, in one aspect, the present disclosure provides a product configured for oral use, the product comprising a mixture comprising one or more particulate filler components, water, one or more organic acids or salts thereof, and one or more flavoring agents, the product having a pH of less than about 7.0.
[0008] In some embodiments, the one or more particulate filler components comprise a cellulosic material. In some embodiments, the cellulosic material comprises microcrystalline cellulose.
[0009] In some embodiments, the one or more particulate filler components further comprise a cellulose derivative in an amount by weight of the mixture of about 1% to about 3%, based on the total weight of the mixture. In some embodiments, the cellulose derivative is hydroxypropyl cellulose. In certain embodiments, the one or more fillers comprise both microcrystalline cellulose (e.g., in an amount of at least about 20% by weight, or at least about 25% by weight, or at least about 30% by weight, based on the weight of the mixture) and a cellulose derivative such as hydroxypropyl cellulose (e.g., in an amount of less than about 5% by weight, or less than about 4% by weight, or less than about 3% by weight, based on the total weight of the mixture).
[0010] In some embodiments, the pH of the mixture is from about 5.5 to about 6.5.
[0011] In some embodiments, the product comprises from about 0.1 to about 10% by weight of one or more organic acids based on the total weight of the mixture, hi some embodiments, the product comprises from about 0.1 to about 0.5% by weight of one or more organic acids based on the total weight of the mixture.
[0012] In some embodiments, the one or more organic acids are alkyl carboxylic acids, aryl carboxylic acids, or combinations thereof. In some embodiments, the one or more organic acids are citric acid, malic acid, tartaric acid, octanoic acid, benzoic acid, toluic acid, salicylic acid, or combinations thereof. In some embodiments, the one or more organic acids are benzoic acid. In some embodiments, the one or more organic acids are citric acid.
[0013] In some embodiments, the product comprises about 10 to about 50% of one or more particulate filler components and about 5 to about 60% by weight of water. In one embodiment, the product comprises about 0.1 to about 10% by weight (e.g., about 0.2 to about 0.5% by weight) of one or more organic acids or salts thereof, a filler (e.g., MCC) in an amount of at least about 30% by weight (e.g., about 30 to about 50% by weight), sodium chloride in an amount of at least about 1% by weight (e.g., about 1 to about 5% by weight), and water in an amount of at least about 30% by weight (e.g., about 35 to about 50% by weight).
[0014] In some embodiments, the mixture further comprises one or more salts, one or more sweeteners, one or more binders, one or more humectants, one or more gums, one or more active ingredients, tobacco materials, or combinations thereof.
[0015] In some embodiments, the mixture further comprises one or more active ingredients selected from the group consisting of a nicotine component, a botanical drug, a stimulant, an amino acid, a vitamin, and a cannabinoid, In some embodiments, the mixture comprises from about 0.001 to about 10% by weight of a nicotine component, calculated as the free base, based on the total weight of the mixture.
[0016] In some embodiments, the flavoring agent comprises a compound having a carbon-carbon double bond, a carbon-oxygen double bond, or both. In some embodiments, the flavoring agent comprises one or more aldehydes, ketones, esters, terpenes, terpenoids, or combinations thereof. In some embodiments, the flavoring agent comprises one or more of ethyl vanillin, cinnamic aldehyde, sabinene, limonene, gamma-terpinene, beta-farnesene, or citral. In some embodiments, the flavoring agent comprises ethyl vanillin.
[0017] In some embodiments, the mixture is enclosed in a pouch to form a pouch product, the mixture optionally being in a free-flowing granular form.
[0018] In some embodiments, the pouch product has one or more of the following when measured at a time period of 1 day after preparation: a whiteness value of greater than about 40 as measured according to the Commission Internationale de l'Eclairage (CIE) model, a delta E (ΔE) value of less than about 4 in the L*a*b* color space as measured with a handheld color meter relative to a control pouch product that does not contain the one or more organic acids, and a concentration of one or more flavoring agents present that is greater than the concentration of the same one or more flavoring agents present in a control pouch product that does not contain the one or more organic acids as measured by semi-quantitative gas chromatography-mass spectrometry. In some embodiments, the whiteness value is from about 42 to about 60. In some embodiments, the ΔE value is from about 0.9 to about 3.8. In some embodiments, the time period is one or more of 2 days, 3 days, 1 week, 2 weeks, 1 month, 2 months, 3 months, 4 months, or 5 months after preparation.
[0019] In another aspect, a method of stabilizing a product configured for oral use is provided, the stabilized product comprising a mixture including one or more particulate filler components, water, one or more organic acids or salts thereof, and one or more flavoring agents, and having a pH of less than about 7.0, the method comprising mixing the one or more particulate filler components with water, the one or more flavoring agents, and the one or more organic acids or salts thereof.
[0020] In some embodiments, the mixing comprises adding one or more organic acids in an amount of about 0.1 to about 10% of the total weight of the mixture. In some embodiments, the mixing comprises adding one or more organic acids in an amount of about 0.1 to about 0.5% of the total weight of the mixture. In some embodiments, the pH of the mixture after the addition is about 5.5 to about 6.5.
[0021] In some embodiments, the one or more organic acids are alkyl carboxylic acids, aryl carboxylic acids, or combinations thereof. In some embodiments, the one or more organic acids are citric acid, malic acid, tartaric acid, octanoic acid, benzoic acid, toluic acid, salicylic acid, or combinations thereof. In some embodiments, the organic acid is benzoic acid. In some embodiments, the organic acid is citric acid.
[0022] In some embodiments, the mixing further comprises adding one or more salts, one or more sweeteners, one or more binders, one or more humectants, one or more gums, one or more active ingredients, tobacco materials, or combinations thereof.
[0023] In some embodiments, the mixing further comprises adding a cellulose derivative in an amount of about 1% to about 3% by weight of the mixture, hi some embodiments, the cellulose derivative is hydroxypropyl cellulose.
[0024] In some embodiments, the mixing further comprises adding one or more active ingredients selected from the group consisting of a nicotine component, a botanical drug, a stimulant, an amino acid, a vitamin, and a cannabinoid.
[0025] In some embodiments, the combining step further comprises adding about 0.001 to about 10% by weight of a nicotine component, calculated as the free base, based on the total weight of the combination.
[0026] In some embodiments, the one or more flavoring agents include at least one volatile component, such as one or more aldehydes, ketones, esters, terpenes, terpenoids, or combinations thereof, In some embodiments, the at least one volatile component includes one or more of ethyl vanillin, sabinene, limonene, gamma-terpinene, beta-farnesene, or citral.
[0027] In some embodiments, the method further comprises enclosing the mixture in a pouch to form a pouch product, the mixture optionally being in free-flowing particle form.
[0028] In some embodiments, when measured at a time period of 1 day after preparation, the stabilized pouch product has one or more of the following: a whiteness value of greater than about 40 when measured according to the Commission Internationale de l'Eclairage (CIE) model, a delta E (ΔE) value of less than about 4 in the L*a*b* color space when measured with a handheld color meter, relative to a control pouch product that does not contain the one or more organic acids, and a concentration of one or more flavoring agents present that is greater than the concentration of the same one or more flavoring agents present in a control pouch product that does not contain the one or more organic acids, as measured by semi-quantitative gas chromatography-mass spectrometry. In some embodiments, the whiteness value is from about 42 to about 60. In some embodiments, the ΔE value is from about 0.9 to about 3.8. In some embodiments, the time period is one or more of 2 days, 3 days, 1 week, 2 weeks, 1 month, 2 months, 3 months, 4 months, or 5 months after preparation.
[0029] In another aspect, there is provided a product adapted for oral use and prepared by the methods disclosed herein.
[0030] In yet another aspect, a pouch product configured for oral use and stabilized against discoloration is provided, the pouch product comprising one or more flavoring agents and having a pH of less than about 7.0. In some embodiments, the pouch product has a whiteness value of greater than about 40 as determined according to the Commission Internationale de l'Eclairage (CIE) model.
[0031] The disclosure includes, but is not limited to, the following embodiments.
[0032] Embodiment 1: A product configured for oral use, comprising a mixture comprising one or more particulate filler ingredients, water, one or more organic acids or salts thereof, and one or more flavoring agents, the product having a pH of less than about 7.0.
[0033] Embodiment 2: The product of embodiment 1, wherein the one or more particulate filler components comprise a cellulosic material.
[0034] Embodiment 3: The product of embodiment 1 or 2, wherein the cellulose material comprises microcrystalline cellulose.
[0035] Embodiment 4: The product of any one of embodiments 1-3, wherein the one or more particulate filler components further comprise a cellulose derivative in an amount of about 1% to about 3% by weight of the mixture.
[0036] Embodiment 5: The product of any one of embodiments 1-4, wherein the cellulose derivative is hydroxypropyl cellulose.
[0037] Embodiment 6: The product of any one of embodiments 1 to 5, wherein the pH of the product is from about 5.5 to about 6.5.
[0038] Embodiment 7: The product of any one of embodiments 1-6, comprising about 0.1 to about 10% by weight of one or more organic acids, based on the total weight of the mixture.
[0039] Embodiment 8: The product of any one of embodiments 1 to 7, comprising about 0.1 to about 0.5 wt. % of one or more organic acids, based on the total weight of the mixture.
[0040] Embodiment 9: The product of any one of embodiments 1-8, wherein the one or more organic acids are alkyl carboxylic acids, aryl carboxylic acids, or any combination thereof.
[0041] Embodiment 10: The product of any one of embodiments 1-9, wherein the one or more organic acids are citric acid, malic acid, tartaric acid, octanoic acid, benzoic acid, toluic acid, salicylic acid, or combinations thereof.
[0042] Embodiment 11: The product of any one of embodiments 1-10, wherein the one or more organic acids is citric acid.
[0043] Embodiment 12: The product of any one of embodiments 1 to 11, comprising about 10 to about 50% of one particulate filler component and about 5 to about 60% by weight of water, based on the total weight of the mixture.
[0044] Embodiment 13: The product of any one of embodiments 1-12, wherein the mixture further comprises one or more salts, one or more sweeteners, one or more binders, one or more humectants, one or more gums, one or more active ingredients, tobacco materials, or combinations thereof.
[0045] Embodiment 14: The product of any one of embodiments 1 to 13, wherein the mixture further comprises one or more active ingredients selected from the group consisting of nicotine components, botanical drugs, stimulants, amino acids, vitamins, and cannabinoids.
[0046] Embodiment 15: The product of any one of embodiments 1 to 14, wherein the mixture comprises from about 0.001 to about 10% by weight of the nicotine component, calculated as the free base, based on the total weight of the mixture.
[0047] Embodiment 16: The product of any one of embodiments 1 to 15, wherein the one or more flavoring agents comprises a compound having a carbon-carbon double bond, a carbon-oxygen double bond, or both.
[0048] Embodiment 17: The product of any one of embodiments 1 to 16, wherein the one or more flavoring agents comprise one or more aldehydes, ketones, esters, terpenes, terpenoids, or combinations thereof.
[0049] Embodiment 18: The product of any one of embodiments 1-17, wherein the one or more flavoring agents include one or more of ethyl vanillin, cinnamaldehyde, sabinene, limonene, gamma-terpinene, beta-farnesene, and citral.
[0050] Embodiment 19: The product of any one of embodiments 1 to 18, wherein the one or more flavoring agents comprises ethyl vanillin.
[0051] Embodiment 20: The product of any one of embodiments 1-19, comprising no more than about 10% by weight of tobacco material, excluding any nicotine components present in the mixture, based on the total weight of the mixture.
[0052] Embodiment 21: The product of any one of embodiments 1 to 20, wherein the mixture is enclosed in a pouch to form a pouch product, and the mixture is optionally in a free-flowing granular form.
[0053] Embodiment 22: The pouch product of any one of embodiments 1-21, wherein when measured at a period of one day after preparation, the stabilized pouch product has one or more of the following: a whiteness value of greater than about 40 when measured according to the Commission Internationale de l'Eclairage (CIE) model; a delta E (ΔE) value of less than about 4 in the L*a*b* color space when measured with a handheld color meter, relative to a control pouch product that does not contain the one or more organic acids; and a concentration of one or more flavoring agents present that is greater than the concentration of the same one or more flavoring agents present in a control pouch product that does not contain the one or more organic acids, as measured by semi-quantitative gas chromatography-mass spectrometry.
[0054] Embodiment 23: The pouch product of any one of embodiments 1 to 22, having a whiteness value of about 42 to about 60.
[0055] Embodiment 24: The pouch product of any one of embodiments 1 to 23, wherein the ΔE value is from about 0.9 to about 3.8.
[0056] Embodiment 25: The pouch product of any one of embodiments 1 to 24, wherein the period is one or more of 2 days, 3 days, 1 week, 2 weeks, 1 month, 2 months, 3 months, 4 months, or 5 months after preparation.
[0057] Embodiment 26: A method of stabilizing a product configured for oral use, wherein the stabilized product comprises a mixture comprising one or more particulate filler components, water, one or more organic acids or salts thereof, and one or more flavoring agents, the method comprising mixing the one or more particulate filler components with water, the one or more flavoring agents, and the one or more organic acids or salts thereof to form a mixture, wherein the mixture has a pH of less than about 7.0.
[0058] Embodiment 27: The method of embodiment 26, wherein the mixing comprises adding one or more organic acids in an amount of about 0.1 to about 10% of the total weight of the mixture.
[0059] Embodiment 28: The method of embodiment 26 or 27, wherein the mixing comprises adding one or more organic acids in an amount of about 0.1 to about 0.5% of the total weight of the mixture.
[0060] Embodiment 29: The method of any one of embodiments 26 to 28, wherein the pH of the product is from about 5.5 to about 6.5.
[0061] Embodiment 30: The method of any one of embodiments 26-29, wherein the one or more organic acids are alkyl carboxylic acids, aryl carboxylic acids, or combinations thereof.
[0062] Embodiment 31: The method of any one of embodiments 26-30, wherein the one or more organic acids are citric acid, malic acid, tartaric acid, octanoic acid, benzoic acid, toluic acid, salicylic acid, or any combination thereof.
[0063] Embodiment 32: The method of any one of embodiments 26-31, wherein the one or more organic acids is citric acid.
[0064] Embodiment 33: The method of any one of embodiments 26-32, wherein the mixing further comprises adding one or more salts, one or more sweeteners, one or more binders, one or more humectants, one or more gums, one or more active ingredients, tobacco materials, or a combination thereof.
[0065] Embodiment 34: The method of any one of embodiments 26 to 33, wherein the mixing further comprises adding a cellulose derivative in an amount of about 1% to about 3% by weight of the mixture.
[0066] Embodiment 35: The method of any one of embodiments 26-34, wherein the cellulose derivative is hydroxypropyl cellulose.
[0067] Embodiment 36: The method of any one of embodiments 26 to 35, wherein the mixing further comprises adding one or more active ingredients selected from the group consisting of a nicotine component, a botanical drug, a stimulant, an amino acid, a vitamin, and a cannabinoid.
[0068] Embodiment 37: The method of any one of embodiments 26-36, wherein the mixing further comprises adding about 0.001 to about 10% by weight of a nicotine component, calculated as the free base, based on the total weight of the mixture.
[0069] Embodiment 38: The method of any one of embodiments 26 to 37, wherein the one or more flavoring agents comprise one or more aldehydes, ketones, esters, terpenes, terpenoids, or combinations thereof.
[0070] Embodiment 39: The method of any one of embodiments 26-38, wherein the one or more flavoring agents comprise one or more of ethyl vanillin, sabinene, limonene, gamma-terpinene, beta-farnesene, and citral.
[0071] Embodiment 40: The method of any one of embodiments 26-39, further comprising encapsulating the mixture in a pouch to form a pouch product, wherein the mixture is in a flowable granular form.
[0072] Embodiment 41: The method of any one of embodiments 26-40, wherein when measured at a period of one day after preparation, the stabilized pouch product has one or more of the following: a whiteness value of greater than about 40 when measured according to the Commission Internationale de l'Eclairage (CIE) model; a delta E (ΔE) value of less than about 4 in the L*a*b* color space when measured with a handheld color meter, relative to a control pouch product that does not contain the one or more organic acids; and a concentration of one or more flavoring agents present that is greater than the concentration of the same one or more flavoring agents present in a control pouch product that does not contain the one or more organic acids, as measured by semi-quantitative gas chromatography-mass spectrometry.
[0073] Embodiment 42: The method of any one of embodiments 26 to 41, wherein the whiteness value is from about 42 to about 60.
[0074] Embodiment 43: The method of any one of embodiments 26 to 42, wherein the ΔE value is from about 0.9 to about 3.8.
[0075] Embodiment 44: The method of any one of embodiments 26 to 43, wherein the period is one or more of 2 days, 3 days, 1 week, 2 weeks, 1 month, 2 months, 3 months, 4 months, or 5 months after preparation.
[0076] Embodiment 45: A product prepared by the method of any one of embodiments 26 to 44, adapted for oral use.
[0077] Embodiment 46: A pouch product adapted for oral use, stabilized against discoloration, comprising one or more flavoring agents, and having a pH of less than about 7.0.
[0078] Embodiment 47: The pouch product of embodiment 46, having a whiteness value of greater than about 40 when measured according to the Commission Internationale de l'Eclairage (CIE) model.
[0079] These and other features, aspects, and advantages of the disclosure will become apparent from a reading of the following detailed description in conjunction with the accompanying figures, which are briefly described below. The present invention includes any combination of two, three, four, or more of the above-described embodiments, as well as any combination of two, three, four, or more features or elements set forth in this disclosure, regardless of whether such features or elements are expressly combined in the description of a particular embodiment herein. This disclosure is intended to be read in its entirety as intended to indicate that all separable features or elements of the disclosed invention are combinable in any of its various aspects and embodiments, unless the context clearly dictates otherwise.
[0080] Having now described aspects of the disclosure in general terms above, reference will now be made to the accompanying drawings, which are not necessarily drawn to scale, which are illustrative only and should not be construed as limiting the disclosure. [Brief description of the drawings]
[0081] [Figure 1] FIG. 1 is a line graph showing pH values versus citric acid concentration for one embodiment. [Diagram 2] Figure 2 shows, from left to right, photographs comparing a control pouch product without flavor with control pouch products containing ethyl vanillin, lime, and cinnamon flavors after 72 hours, one week, and one month, respectively. [Diagram 3] FIG. 3 is a photograph of an embodiment containing ethyl vanillin and an organic acid compared to a control pouch product containing no organic acid after 72 hours. [Figure 4] FIG. 4 is a line graph showing ΔE values versus organic acid concentration for embodiments including ethyl vanillin. [Diagram 5] FIG. 5 is a photograph of an embodiment containing a terpene component and an organic acid compared to a control pouch product containing no organic acid after approximately one week. [Figure 6] FIG. 6 is a line graph showing ΔE values versus organic acid concentration for embodiments including lime flavoring, which includes terpenes. [Figure 7] FIG. 7 is a bar graph showing subjective overall taste intensity versus organic acid concentration for embodiments including lime flavoring, including terpenes. [Figure 8] FIG. 8 is a bar graph showing subjective citrus taste intensity versus organic acid concentration for embodiments including lime flavoring, including terpenes. [Figure 9] FIG. 9 is a cross-sectional view of an embodiment of a pouch product taken across the width of the product, showing the outer pouch filled with a mixture of the present disclosure. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0082] The present disclosure provides products that exhibit enhanced flavor and / or color stability, and methods for stabilizing flavor components in such products. For customer satisfaction, it is desirable to provide products that are suitable for oral use that retain certain initial properties, such as whiteness and flavor profile. Surprisingly, in accordance with the present disclosure, in certain embodiments, it has been found that the addition of one or more organic acids to a mixture results in a product that exhibits improved stability of certain properties relative to a product containing the mixture without the one or more organic acids. In particular, it has been found that the presence of an organic acid in the range of about 0.1 to about 10% by weight in a mixture as disclosed herein prevents products containing such mixtures from darkening rapidly and / or gradually, and in some embodiments, prevents the loss of certain volatile flavor components in such products.
[0083] The present disclosure will now be described more fully below with reference to exemplary embodiments thereof. These exemplary embodiments are described so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art. Indeed, the disclosure may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather, these embodiments are provided so that this disclosure will satisfy applicable legal requirements. As used in this specification and the claims, the singular forms "a," "an," and "the" include plural referents unless the context clearly dictates otherwise. References to "dry weight percent" or "dry weight basis" refer to weight based on dry ingredients (i.e., all ingredients excluding water). References to "wet weight" refer to the weight of the mixture, including water. Unless otherwise specified, references to "weight percent" of a mixture reflect the total wet weight of the mixture (i.e., including water).
[0084] The products described herein include a mixture comprising one or more particulate filler components, one or more organic acids or salts thereof, and one or more flavoring agents. In some embodiments, the mixture further comprises one or more salts, one or more sweeteners, one or more binders, one or more humectants, one or more gums, one or more active ingredients, tobacco materials, tobacco-derived materials, or combinations thereof. The relative amounts of the various components in the mixture may vary, but are typically selected to provide the oral product with the desired sensory and performance characteristics. Exemplary individual components of the mixture are described below.
[0085] <Filler components> The mixtures described herein include at least one particulate filler component. Such particulate filler components can perform multiple functions, such as enhancing certain sensory properties, such as texture and mouthfeel, and increasing the cohesiveness or compressibility of the product. In general, the filler component is a porous particulate material and is based on cellulose. For example, suitable particulate filler components are any non-tobacco plant material or derivatives thereof, including cellulose materials derived from such sources. Examples of cellulosic non-tobacco plant materials include grains (e.g., corn, oat, barley, rye, buckwheat, etc.), sugar beet (e.g., FIBREX® brand filler available from International Fiber Corporation), bran fiber, and mixtures thereof. Non-limiting examples of derivatives of non-tobacco plant materials include starch (e.g., from potato, wheat, rice, corn), natural cellulose, and modified cellulose materials. Further examples of potential particulate filler components include maltodextrin, dextrose, calcium carbonate, calcium phosphate, lactose, mannitol, xylitol, and sorbitol. Combinations of fillers may also be used.
[0086] As used herein, "starch" can refer to pure starch, modified starch, or starch derivatives from any source. Starch, typically in granular form, is present in almost all green plants and in various types of plant tissues and organs (e.g., seeds, leaves, rhizomes, roots, tubers, shoots, fruits, grains, stems). Starch varies in composition as well as in granular shape and size. Starches from different sources often have different chemical and physical properties. A particular starch can be selected for inclusion in the mixture based on the ability of the starch material to impart specific sensory properties to the composition. Starches from various sources can be used. For example, major sources of starch include cereals (e.g., rice, wheat, and corn) and root vegetables (e.g., potato and cassava). Other examples of sources of starch include acorns, arrowroot, arracacha, banana, barley, legumes (e.g., broad bean, lentil, mung bean, pea, chickpea), breadfruit, buckwheat, canna, chestnut, taro, dogtooth violet, kudzu, malanga, millet, oats, oka, Polynesian arrowroot, sago palm, sorghum, sweet potato, quinoa, rye, tapioca, taro, tobacco, water chestnut, and yam. Certain starches are modified starches. Modified starches have undergone one or more structural modifications, often designed to alter their high thermal properties. Some starches have been developed by genetic engineering and are considered "modified" starches. Other starches are modified after they are obtained. For example, modified starches can be starches that have been subjected to chemical reactions such as esterification, etherification, oxidation, depolymerization (thinning), bleaching, transglycosylation and depolymerization (e.g., dextrinization in the presence of a catalyst), crosslinking, enzyme treatment, acetylation, hydroxypropylation, and / or partial hydrolysis by acid catalysis or oxidation in the presence of a base. Other starches are modified by heat treatment, e.g., pregelatinization, dextrinization, and / or cold water swelling methods.Specific modified starches include monostarch phosphate, distarch glycerol, distarch phosphate esterified with sodium trimetaphosphate, distarch phosphate, acetylated crosslinked starch phosphate, starch acetate esterified with acetic anhydride, starch acetate esterified with vinyl acetate, acetylated crosslinked starch adipate, acetylated distarch glycerol, hydroxypropyl starch, hydroxypropyl distarch glycerol, and sodium starch octenyl succinate.
[0087] In some embodiments, the particulate filler component is a cellulose material or a cellulose derivative. One particularly suitable particulate filler component for use in the products described herein is microcrystalline cellulose ("mcc"). mcc can be synthetic, semi-synthetic, or derived entirely from natural cellulose. mcc can be selected from the group consisting of AVICEL® grades PH-100, PH-102, PH-103, PH-105, PH-112, PH-113, PH-200, PH-300, PH-302, VIVACEL® grades 101, 102, 12, 20, and EMOCEL® grades 50M and 90M, and the like, and mixtures thereof. In one embodiment, the mixture includes mcc as a particulate filler component. The amount of mcc present in the mixture as described herein can vary according to the desired properties.
[0088] The amount of the particulate filler component can vary, but is typically up to about 75 weight percent of the mixture based on the total weight of the mixture. A typical range of particulate filler material (e.g., mcc) in the mixture can be from about 10 to about 75 weight percent, e.g., from about 10, about 15, about 20, about 25, or about 30 to about 35, about 40, about 45, or about 50 weight percent (e.g., about 20 to about 50 weight percent or about 25 to about 45 weight percent) of the total weight of the mixture. In certain embodiments, the amount of particulate filler material is at least about 10 weight percent, e.g., at least about 20 weight percent, or at least about 25 weight percent, or at least about 30 weight percent, or at least about 35 weight percent, or at least about 40 weight percent, based on the total weight of the mixture.
[0089] In one embodiment, the particulate filler component further comprises a cellulose derivative or a combination of such derivatives. In some embodiments, the mixture comprises about 1 to about 10 wt. % of the cellulose derivative, and certain embodiments comprise about 1 to about 5 wt. % of the cellulose derivative, based on the total weight of the mixture. In certain embodiments, the cellulose derivative is a cellulose ether (including a carboxyalkyl ether), which refers to a cellulose polymer having one or more hydroxyl hydrogens in the cellulose structure substituted with an alkyl group, a hydroxyalkyl group, or an aryl group. Non-limiting examples of such cellulose derivatives include methylcellulose, hydroxypropylcellulose ("HPC"), hydroxypropylmethylcellulose ("HPMC"), hydroxyethylcellulose, and carboxymethylcellulose ("CMC"). In one embodiment, the cellulose derivative is one or more of methylcellulose, HPC, HPMC, hydroxyethylcellulose, and CMC. In one embodiment, the cellulose derivative is HPC. In some embodiments, the mixture comprises about 1 to about 3 wt. % of HPC, based on the total weight of the mixture.
[0090] <Water> The water content of the mixture in the product can vary according to the desired properties prior to consumer use of the product. Typically, the mixture is less than about 60 percent water by weight, generally about 1 to about 60 percent water by weight, such as about 5 to about 55, about 10 to about 50, about 20 to about 45, or about 25 to about 40 percent water by weight, including amounts of water of at least about 5%, at least about 10%, at least about 15%, and at least about 20% by weight, as present in the product prior to insertion into the user's mouth.
[0091] <Organic acid> As used herein, the term "organic acid" refers to an organic (i.e., carbon-based) compound characterized by acidic properties. Typically, organic acids are carboxylic acids (-CO 2 The organic acids are relatively weak acids (i.e., do not completely dissociate in the presence of water), such as sulfonic acids (-SOOH) or sulfuric acids (-SOOH). As used herein, reference to an organic acid means an organic acid that is intentionally added. In this regard, the organic acid may be intentionally added as a particular mixture component, as opposed to merely being inherently present as a component of another mixture component (e.g., small amounts of organic acids that may be inherently present in a mixture component such as a tobacco material). In some embodiments, the one or more organic acids are added neat (i.e., in their free acid, natural solid or liquid form) or as a solution, for example, in water. In some embodiments, the one or more organic acids are added in the form of a salt, as described below.
[0092] Suitable organic acids are typically those that have a range of lipophilicity (i.e., polarity that provides an appropriate balance of aqueous and organic solubility). Lipophilicity is conveniently measured in terms of logP, the partition coefficient of a molecule between an aqueous phase and an oleophilic phase (usually water and octanol). Typically, the lipophilicity of an organic acid may be between about -2 and about 6.5. In some embodiments, the organic acid may be more soluble in water than in octanol (i.e., has a negative logP value, such as about -2 to about -1). In some embodiments, the organic acid may be about equally soluble in water and octanol (i.e., has a logP value of about 0). In some embodiments, the organic acid may be more soluble in octanol than in water (i.e., has a positive logP value, such as about 1 to about 6.5). In some embodiments, the organic acid has a logP value of about 1.5 to about 5.0, such as from about 1.5, about 2.0, about 2.5, or about 3.0 to about 3.5, about 4.0, about 4.5, or about 5.0.
[0093] In some embodiments, the organic acid is a carboxylic acid or a sulfonic acid. The carboxylic acid or sulfonic acid functional group may, for example, be an organic acid having 1 to 20 carbon atoms (C1 to C 20 ) can be attached to any alkyl, cycloalkyl, heterocycloalkyl, aryl, or heteroaryl group. In some embodiments, the organic acid is an alkyl, cycloalkyl, heterocycloalkyl, aryl, or heteroaryl carboxylic or sulfonic acid.
[0094] As used herein, "alkyl" refers to any straight or branched chain hydrocarbon. The alkyl group may be saturated (i.e., all sp 3 As used herein, the term "unsaturated" refers to a carbon-carbon, sp , or cyclic alkyl group at one or more positions within an alkyl group. 2It refers to the presence of a double bond. Unsaturated alkyl groups may be monounsaturated or polyunsaturated. Representative straight chain alkyl groups include, but are not limited to, methyl, ethyl, n-propyl, n-butyl, n-pentyl, and n-hexyl. Branched chain alkyl groups include, but are not limited to, isopropyl, sec-butyl, isobutyl, tert-butyl, isopentyl, and 2-methylbutyl. Representative unsaturated alkyl groups include, but are not limited to, ethylene or vinyl, allyl, 1-butenyl, 2-butenyl, isobutylenyl, 1-pentenyl, 2-pentenyl, 3-methyl-1-butenyl, 2-methyl-2-butenyl, 2,3-dimethyl-2-butenyl, and the like. Alkyl groups may be unsubstituted or substituted.
[0095] As used herein, "cycloalkyl" refers to a carbocyclic group, which may be monocyclic or bicyclic. Cycloalkyl groups include rings having 3 to 7 carbon atoms as a monocycle, or 7 to 12 carbon atoms as a bicycle. Examples of monocyclic cycloalkyl groups include cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, cycloheptyl, and cyclooctyl. Cycloalkyl groups may be unsubstituted or substituted and may contain one or more sites of unsaturation (e.g., cyclopentenyl or cyclohexenyl).
[0096] The term "aryl" as used herein refers to a carbocyclic aromatic group. Examples of aryl groups include, but are not limited to, phenyl and naphthyl. Aryl groups can be unsubstituted or substituted.
[0097] As used herein, "heteroaryl" and "heterocycloalkyl" refer to an aromatic or non-aromatic ring system in which one or more ring atoms are heteroatoms, e.g., nitrogen, oxygen, and sulfur, respectively. A heteroaryl or heterocycloalkyl group contains up to 20 carbon atoms and 1-3 heteroatoms selected from N, O, and S. A heteroaryl or heterocycloalkyl group can be a monocyclic ring having 3-7 ring members (e.g., 2-6 carbon atoms and 1-3 heteroatoms selected from N, O, and S), or a bicyclic ring having 7-10 ring members (e.g., 4-9 carbon atoms and 1-3 heteroatoms selected from N, O, and S), e.g., a bicyclo[4,5], [5,5], [5,6], or [6,6] system. Examples of heteroaryl groups include pyridyl, thiazolyl, tetrahydrothiophenyl, pyrimidinyl, furanyl, thienyl, pyrrolyl, pyrazolyl, imidazolyl, tetrazolyl, benzofuranyl, thianaphthalenyl, indolyl, indolenyl, quinolinyl, isoquinolinyl, benzimidazolyl, isoxazolyl, pyrazinyl, pyridazinyl, indolizinyl, isoindolyl, 3H-indolyl, 1H-indazolyl, purinyl, 4H-quinolizinyl, and phthalazinyl. , naphthyridinyl, quinoxalinyl, quinazolinyl, cinnolinyl, pteridinyl, 4aH-carbazolyl, carbazolyl, phenanthridinyl, acridinyl, pyrimidinyl, phenanthrolinyl, phenazinyl, phenothiazinyl, furazanyl, phenoxazinyl, isochromanyl, chromanyl, imidazolidinyl, imidazolinyl, pyrazolidinyl, pyrazolinyl, benzotriazolyl, benzisoxazolyl and isatinoyl. Examples of heterocycloalkyl include, but are not limited to, dihydropyridyl, tetrahydropyridyl (piperidyl), tetrahydrothiophenyl, piperidinyl, 4-piperidonyl, pyrrolidinyl, 2-pyrrolidonyl, tetrahydrofuranyl, tetrahydropyranyl, bis-tetrahydropyranyl, tetrahydroquinolinyl, tetrahydroisoquinolinyl, decahydroquinolinyl, octahydroisoquinolinyl, piperazinyl, quinuclidinyl, and morpholinyl.The heteroaryl and heterocycloalkyl groups can be unsubstituted or substituted.
[0098] As used herein, and as applied to any of the above alkyl, aryl, cycloalkyl, heteroaryl, and heterocyclyl, "substituted" means that one or more hydrogen atoms are each independently replaced with a substituent. Exemplary substituents include, but are not limited to, qw-Cl, Br, F, alkyl, -OH, -OCH3, NH2, -NHCH3, -N(CH3)2, -CN, -NC(=O)CH3, -C(=O)-, -C(=O)NH2, and C(=O)N(CH3)2. When a group is described as "optionally substituted," the group may be substituted with one or more of the above substituents, each independently selected. In some embodiments, the substituent may be one or more methyl groups or one or more hydroxyl groups.
[0099] In some embodiments, the organic acid is an alkyl carboxylic acid. Non-limiting examples of alkyl carboxylic acids include formic acid, acetic acid, propionic acid, octanoic acid, nonanoic acid, decanoic acid, undecanoic acid, dodecanoic acid, stearic acid, oleic acid, linoleic acid, linolenic acid, and the like. In some embodiments, the organic acid is an alkyl sulfonic acid. Non-limiting examples of alkyl sulfonic acids include propane sulfonic acid and octane sulfonic acid.
[0100] In some embodiments, the alkyl carboxylic or alkyl sulfonic acids are substituted with one or more hydroxyl groups. Non-limiting examples include glycolic acid, 4-hydroxybutyric acid, and lactic acid.
[0101] In some embodiments, the organic acid can contain more than one carboxylic acid group or more than one sulfonic acid group (e.g., two, three, or more carboxylic acid groups). Non-limiting examples include oxalic acid, fumaric acid, maleic acid, and glutaric acid. In organic acids containing multiple carboxylic acids (e.g., two to four carboxylic acid groups), one or more of the carboxylic acid groups may be esterified. Non-limiting examples include succinic acid monoethyl ester, monomethyl fumarate, monomethyl citrate, or dimethyl citrate, etc.
[0102] In some embodiments, the organic acid can contain more than one carboxylic acid group and more than one hydroxyl group. Non-limiting examples of such acids include tartaric acid, citric acid, and the like.
[0103] In some embodiments, the organic acid is an aryl carboxylic acid or aryl sulfonic acid. Non-limiting examples of aryl carboxylic and aryl sulfonic acids include benzoic acid, toluic acid, salicylic acid, benzenesulfonic acid, and p-toluenesulfonic acid.
[0104] Further non-limiting examples of suitable organic acids include 2,2-dichloroacetic acid, 2-hydroxyethanesulfonic acid, 2-oxoglutaric acid, 4-acetamidobenzoic acid, 4-aminosalicylic acid, acetic acid, adipic acid, ascorbic acid (L), camphoric acid (+), camphor-10-sulfonic acid (+), capric acid, caproic acid, caprylic acid, cinnamic acid, cyclamic acid, decanoic acid, dodecylsulfuric acid, ethane-1,2-disulfonic acid, ethanes ... Examples of acids that may be used include carboxylic acid, formic acid, fumaric acid, galactaric acid, gentisic acid, glucoheptonic acid, gluconic acid, glucuronic acid, glutamic acid, glycerophosphoric acid, glycolic acid, hippuric acid, isobutyric acid, lactobionic acid, lauric acid, malonic acid, mandelic acid, methanesulfonic acid, naphthalene-1,5-disulfonic acid, naphthalene-2-sulfonic acid, oleic acid, palmitic acid, pamoic acid, pyroglutamic acid, sebacic acid, stearic acid, and undecylenic acid.
[0105] In some embodiments, the one or more organic acids is a single organic acid, hi some embodiments, the one or more organic acids is a combination of several acids, such as two, three, or more organic acids.
[0106] In some embodiments, the organic acid is citric acid, malic acid, tartaric acid, octanoic acid, benzoic acid, toluic acid, salicylic acid, or a combination thereof. In some embodiments, the organic acid is benzoic acid. In some embodiments, the organic acid is citric acid.
[0107] In alternative embodiments, some or even all of the organic acid can be added in the form of a salt with an alkaline component, which can include, but is not limited to, nicotine. For example, non-limiting examples of suitable salts for nicotine include formate, acetate, propionate, isobutyrate, butyrate, alpha-methylbutyrate, isovalerate, β-methylvalerate, caproate, 2-furoate, phenylacetate, heptanoate, octanoate, nonanoate, oxalate, malonate, glycolate, benzoate, tartrate, levulinate, ascorbate, fumarate, citrate, malate, lactate, aspartate, salicylate, tosylate, succinate, and pyruvate. In some embodiments, the organic acid or a portion thereof can be added in the form of a salt with an alkali metal, such as sodium, potassium, etc. In organic acids having more than one acid group (such as dicarboxylic acid or tricarboxylic acid), in some cases, one or more of these acid groups can be in such a salt form. Suitable non-limiting examples include monosodium citrate, disodium citrate, etc. In some embodiments, the organic acid is a salt of citric acid, malic acid, tartaric acid, octanoic acid, benzoic acid, toluic acid, salicylic acid, or combinations thereof. In some embodiments, the organic acid is a mono- or di-ester of a di- or tricarboxylic acid, such as the monomethyl ester of citric acid, malic acid, or tartaric acid, or the dimethyl ester of citric acid, respectively.
[0108] The amount of organic acid present in the mixture can vary. Generally, the mixture comprises about 0.1 to about 10% by weight of organic acid present as one or more organic acids based on the total weight of the mixture. In some embodiments, the mixture comprises about 0.1%, about 0.2%, about 0.3%, about 0.4%, about 0.5%, about 0.6%, about 0.7%, about 0.8%, about 0.9%, about 1%, about 2%, about 3%, about 4%, about 5%, about 6%, about 7%, about 8%, about 9%, or about 10% of organic acid based on the total weight of the mixture. In some embodiments, the mixture comprises about 0.1 to about 0.5% by weight, e.g., about 0.1, about 0.15, about 0.2, about 0.25, about 0.3, about 0.35, about 0.4, about 0.45, or about 0.5% by weight of organic acid based on the total weight of the mixture. In some embodiments, the mixture comprises from about 0.25 to about 0.35 weight percent, e.g., from about 0.25, about 0.26, about 0.27, about 0.28, about 0.29, or about 0.3, to about 0.31, about 0.32, about 0.33, about 0.34, or about 0.35 weight percent of an organic acid based on the total weight of the mixture. If a salt of an organic acid is added, the weight percentage is calculated based on the weight of the free acid, not including any counterion that may be present.
[0109] The amount of acid present will vary based on the acidity and basicity of other components (e.g., nicotine, salts, buffers, etc.) that may be present in the mixture. Thus, the organic acid is provided in an amount sufficient to provide a pH of the mixture of 7.0 or less (typically about 6.8 or less, about 6.6 or less, or about 6.5 or less). In certain embodiments, the inclusion of the acid is sufficient to provide a pH of the mixture of about 4.0 to about 7.0, e.g., about 4.5, about 5.0, about 5.5, or about 6.0 to about 6.5, or about 7.0. In some embodiments, the organic acid is provided in an amount sufficient to provide a pH of the mixture of about 5.5 to about 6.5, e.g., about 5.5, about 5.6, about 5.7, about 5.8, about 5.9, or about 6.0 to about 6.1, about 6.2, about 6.3, about 6.4, or about 6.5.
[0110] <Flavoring agent> As used herein, a "flavoring agent" or "flavorant" is any flavorful, aromatic substance capable of altering the sensory properties associated with an oral product. Examples of sensory properties that may be modified by a flavoring agent include taste, mouthfeel, moistness, cool / heat, and / or flavor / aroma. Flavoring agents may be natural or synthetic, and the flavor characteristics imparted thereby may be described, without limitation, as fresh, sweet, herbal, confectionery, floral, fruity, or spicy. Specific types of flavors include, but are not limited to, vanilla, coffee, chocolate / cocoa, cream, mint, spearmint, menthol, peppermint, wintergreen, eucalyptus, lavender, cardamom, nutmeg, cinnamon, clove, cascarilla, sandalwood, honey, ginger, anise, sage, licorice, lemon, orange, apple, peach, lime, cherry, strawberry, and any combination thereof. See also Leffingwell et al., Tobacco Flavoring for Smoking Products, R. J. Reynolds Tobacco Company (1972), incorporated herein by reference. Flavoring agents may also include ingredients that are considered humectants, coolants, or smoothing agents, such as eucalyptus. These flavors may be provided solvent-free (i.e., alone) or in combination and employed as concentrates or flavor packages (e.g., spearmint and menthol, orange and cinnamon, lime, pineapple, etc.). Representative types of ingredients are also described in U.S. Pat. No. 5,387,416 to White et al., U.S. Patent Application Publication No. 2005 / 0244521 to Strickland et al., and PCT International Publication No. WO 05 / 041699 to Quinter et al., each of which is incorporated herein by reference. In some cases, flavoring agents may be provided in spray-dried or liquid form.
[0111] Flavoring agents generally include at least one volatile flavor ingredient. As used herein, "volatile" refers to chemicals that readily form vapors at ambient temperatures (i.e., chemicals that have a high vapor pressure at a given temperature relative to non-volatile substances). Typically, volatile flavor ingredients have a molecular weight of less than about 400 Da and often contain at least one carbon-carbon double bond, carbon-oxygen double bond, or both. In one embodiment, the at least one volatile flavor ingredient includes one or more alcohols, aldehydes, aromatic hydrocarbons, ketones, esters, terpenes, terpenoids, or combinations thereof. Non-limiting examples of aldehydes include vanillin, ethyl vanillin, p-anisaldehyde, hexanal, furfural, isovaleraldehyde, cuminaldehyde, benzaldehyde, and citronellal. Non-limiting examples of ketones include 1-hydroxy-2-propanone and 2-hydroxy-3-methyl-2-cyclopentenone-1-one. Non-limiting examples of esters include allyl hexanoate, ethyl heptanoate, ethyl hexanoate, isoamyl acetate, and 3-methylbutyl acetate. Non-limiting examples of terpenes include sabinene, limonene, gamma-terpinene, beta-farnesene, nerolidol, thujone, myrcene, geraniol, nerol, citronellol, linalool, and eucalyptol. In one embodiment, the at least one volatile flavor component comprises one or more of ethyl vanillin, cinnamic aldehyde, sabinene, limonene, gamma-terpinene, beta-farnesene, or citral. In one embodiment, the at least one volatile flavor component comprises ethyl vanillin.
[0112] The amount of flavorant utilized in the mixture can vary, but is typically up to about 10 weight percent, with certain embodiments characterized by a flavorant content of at least about 0.1 weight percent, e.g., from about 0.5 to about 10 weight percent, from about 1 to about 6 weight percent, or from about 2 to about 5 weight percent, based on the total weight of the mixture.
[0113] The amount of flavoring agent present in the mixture may change over a period of time (e.g., during storage after preparation of the mixture). For example, certain volatile components present in the mixture may evaporate or undergo chemical transformation, resulting in a decrease in the concentration of one or more volatile aroma components. In one embodiment, the concentration of one or more of the at least one volatile flavoring components present is higher than the concentration of the same one or more volatile flavoring components present in a control pouch product that does not contain one or more organic acids after the same period of time. Without wishing to be bound by theory, it is believed that the same mechanism that causes the loss of whiteness gradually reduces certain volatile components (e.g., aldehydes, ketones, terpenes) in the flavoring agent. Thus, the decrease in the presence of these volatile components that lead to discoloration over time can be expected to reduce the sensory satisfaction associated with products that undergo such deterioration processes.
[0114] <Salt> In some embodiments, the mixture may further include a salt typically used in an amount sufficient to provide the mixture with desired sensory attributes (e.g., an alkali metal salt). Non-limiting examples of suitable salts include sodium chloride, potassium chloride, ammonium chloride, flour salt, and the like. When present, a representative amount of salt is about 0.5 weight percent or more, about 1.0 weight percent or more, or about 1.5 weight percent or more of the total weight of the mixture, but typically comprises about 10 weight percent or less, or about 7.5 weight percent or less, or about 5 weight percent or less (e.g., about 0.5 to about 5 weight percent).
[0115] <Sweetener> The mixture typically further comprises one or more sweeteners. The sweetener can be any sweetener or combination of sweeteners, in natural or artificial form, or a combination of natural and artificial sweeteners. Examples of natural sweeteners include fructose, sucrose, glucose, maltose, mannose, galactose, lactose, stevia, honey, etc. Examples of artificial sweeteners include sucralose, isomaltulose, maltodextrin, saccharin, aspartame, acesulfame K, neotame, etc. In some embodiments, the sweetener comprises one or more sugar alcohols. Sugar alcohols are polyols derived from mono- or disaccharides, with partial or complete hydrogenation. Sugar alcohols, for example, have from about 4 to about 20 carbon atoms and include erythritol, arabitol, ribitol, isomalt, maltitol, dulcitol, iditol, mannitol, xylitol, lactitol, sorbitol, and combinations thereof (e.g., hydrogenated starch hydrolysates).When present, representative amounts of sweeteners, on a weight basis, may comprise from about 0.1 to about 20 weight percent or more of the mixture, for example, from about 0.1 to about 1%, from about 1 to about 5%, from about 5 to about 10%, or from about 10 to about 20% of the mixture.
[0116] <Binding agent> A binder (or combination of binders) may be used in certain embodiments in an amount sufficient to provide the mixture with the desired physical attributes and physical integrity. Exemplary binders may be organic or inorganic, or combinations thereof. Exemplary binders include povidone, sodium alginate, starch-based binders, pectin, carrageenan, pullulan, zein, and the like, and combinations thereof. A binder may be used in an amount sufficient to provide the mixture with the desired physical attributes and physical integrity. The amount of binder utilized in the mixture may vary, but is typically up to about 30 weight percent, with certain embodiments characterized by a binder content of at least about 0.1 weight percent, e.g., from about 1 to about 30 weight percent, or from about 5 to about 10 weight percent, based on the total weight of the mixture.
[0117] In certain embodiments, the binder comprises a gum, e.g., a natural gum. As used herein, a natural gum refers to a polysaccharide material of natural origin that has binding properties and is also useful as a thickening or gelling agent. Representative natural gums derived from plants are typically water-soluble to some extent and include xanthan gum, guar gum, gum arabic, gum ghatti, gum tragacanth, gum karaya, locust bean gum, gellan gum, and combinations thereof. When present, the natural gum binder material is typically present in an amount of up to about 5% by weight, e.g., from about 0.1, about 0.2, about 0.3, about 0.4, about 0.5, about 0.6, about 0.7, about 0.8, about 0.9, or about 1% by weight to about 2%, about 3%, about 4%, or about 5% by weight, based on the total weight of the mixture.
[0118] <Wetting agent> In certain embodiments, one or more humectants may be used in the mixture. Examples of humectants include, but are not limited to, glycerin, propylene glycol, and the like. If included, the humectant is typically provided in an amount sufficient to provide the mixture with desired moisture attributes. Additionally, in some cases, the humectant may impart desirable flow properties to the mixture for deposition into a mold. If present, the humectant typically comprises about 5% or less of the weight of the mixture (e.g., about 0.5 to about 5% by weight). If present, a representative amount of humectant is about 0.1% to about 1% by weight, or about 1% to about 5% by weight, based on the total weight of the mixture.
[0119] <Buffer> In certain embodiments, the mixture of the present disclosure may include a pH adjuster or buffering agent. Examples of pH adjusters and buffering agents that can be used include, but are not limited to, metal hydroxides (e.g., alkali metal hydroxides such as sodium hydroxide and potassium hydroxide), and metal carbonates (e.g., potassium carbonate or sodium carbonate), or other alkali metal buffers such as metal bicarbonates such as sodium bicarbonate. When present, the buffering agent is typically present in an amount of less than about 5% based on the weight of the mixture, for example, about 0.5% to about 5% by weight, for example, about 0.75% to about 4% by weight, about 0.75% to about 3% by weight, or about 1% to about 2% by weight based on the total weight of the mixture. Non-limiting examples of suitable buffering agents include alkali metal acetates, glycinates, phosphates, glycerophosphates, citrates, carbonates, bicarbonates, borates, or mixtures thereof.
[0120] <Coloring agent> Colorants may be used in amounts sufficient to provide the mixture with desired physical attributes. Examples of colorants include various dyes and pigments, such as caramel color and titanium dioxide. The amount of colorant utilized in the mixture may vary, but when present, is typically up to about 3% by weight, for example, about 0.1%, about 0.5%, or about 1% to about 3% by weight, based on the total weight of the mixture.
[0121] <Active ingredient> The mixture may further include one or more active ingredients, including, but not limited to, a nicotine component, a botanical component (such as lavender, peppermint, chamomile, basil, rosemary, ginger, cannabis, ginseng, maca, tisane, etc.), a stimulant (such as caffeine, guarana, etc.), an amino acid (such as taurine, theanine, phenylalanine, tyrosine, tryptophan, etc.), and / or a pharmaceutical, nutraceutical, and / or medicinal component (such as vitamins, e.g., B6, B12, C, etc., and / or cannabinoids, such as tetrahydrocannabinol (THC) and cannabidiol (CBD)). The particular percentages and selection of ingredients will vary depending on the flavor, texture, and other characteristics desired. For example, an active ingredient would include any ingredient known to affect one or more biological functions in the body, such as ingredients that provide pharmacological activity or other direct effect in the diagnosis, cure, mitigation, treatment, or prevention of disease, or that affect the structure or any function of the human or other animal body (e.g., providing a stimulating effect on the central nervous system, having an energizing effect, having an antipyretic or analgesic effect, or having an otherwise useful effect on the body).
[0122] In certain embodiments, a nicotine component can be included in the mixture. By "nicotine component" is meant any suitable form of nicotine (e.g., free base or salt) to provide oral absorption of at least a portion of the nicotine present. Typically, the nicotine component is selected from the group consisting of nicotine free base and nicotine salt. In some embodiments, nicotine is in its free base form, which can be easily adsorbed, for example, into microcrystalline cellulose material to form a microcrystalline cellulose-nicotine carrier complex. See, for example, the discussion of nicotine in free base form in Hansson, US Patent Application Publication No. 2004 / 0191322, incorporated herein by reference.
[0123] In some embodiments, at least a portion of the nicotine may be used in the form of a salt. The nicotine salt may be provided using the types of ingredients and techniques described in U.S. Patent No. 2,033,909 to Cox et al. and Perfetti, Beitrage Tabakforschung Int., 12:43-54 (1983), which are incorporated herein by reference. Additionally, nicotine salts may be obtained from sources such as Pfaltz and Bauer, Inc. and K&K Laboratories, a division of ICN Biochemicals, Inc. Typically, the nicotine ingredient is selected from the group consisting of nicotine salts such as nicotine free base, hydrochloride, dihydrochloride, monotartrate, bitartrate, sulfate, salicylate, and nicotine zinc chloride. In some embodiments, the nicotine ingredient or a portion thereof is a nicotine salt with at least a portion of one or more organic acids disclosed herein.
[0124] In some embodiments, at least a portion of the nicotine may be in the form of a resin complex of nicotine, where the nicotine is bound to an ion exchange resin, such as nicotine polacrilex bound to a polymethacrylic acid, such as Amberlite IRP64, Purolite C115HMR, or Doshion P551. See, for example, U.S. Patent No. 3,901,248 to Lichtneckert et al., incorporated herein by reference. Another example is a nicotine-polyacryl carbomer complex, such as with Carbopol 974P. In some embodiments, the nicotine may be present in the form of a nicotine polyacryl complex.
[0125] Typically, the nicotine component, when present, (calculated as the free base), is at a concentration of at least about 0.001% by weight of the mixture, e.g., in the range of about 0.001% to about 10%. In some embodiments, the nicotine component, calculated as the free base, is present in a concentration of from about 0.1% w / w to about 10% by weight, e.g., from about 0.1% w / w, about 0.2% w / w, about 0.3% w / w, about 0.4% w / w, about 0.5% w / w, about 0.6% w / w, about 0.7% w / w, about 0.8% w / w, or about 0.9% w / w to about 1% w / w, about 2% w / w, about 3% w / w, about 4% w / w, about 5% w / w, about 6% w / w, about 7% w / w, about 8% w / w, about 9% w / w, or about 10% w / w, based on the total weight of the mixture. In some embodiments, the nicotine component is present in a concentration of about 0.1% w / w to about 3% by weight, calculated as the free base, based on the total weight of the mixture, e.g., from about 0.1% w / w to about 2.5%, from about 0.1% to about 2.0%, from about 0.1% to about 1.5%, or from about 0.1% to about 1% by weight. These ranges are also applicable to other active ingredients described herein.
[0126] Tobacco Materials In some embodiments, the mixture can include tobacco material. The tobacco material can vary in species, variety, and form. Generally, the tobacco material is obtained from harvested plants of the Nicotiana species. Examples of Nicotiana species include N. tabacum, N. rustica, N. alata, N. arentsii, N. excelsior, N. forgetiana, N. glauca, N. glutinosa, N. gossei, N. kawakamii, N. knightiana, N. langsdorffi, N. otophora, N. setchelli, N. sylvestris, N. tomentosa, N. tomentosiformis, N. undulata, Nx sanderae, N. africana, N. amplexicaulis, N. benavidesii, N. bonariensis, N. debneyi, N. longiflora, N. maritina, N. megalosiphon, N. occidentalis, N. paniculata, N. plumbaginifolia , N. raimondii, N. rosulata, N. simulans, N. stocktonii, N. suaveolens, N. umbratica, N. velutina, N. wigandioides, N. acaulis, N. acuminata, N. attenuata, N. benthamiana, N. cavicola, N.These include N. clevelandii, N. cordifolia, N. corymbosa, N. fragrans, N. goodspeedii, N. linearis, N. miersii, N. nudicaulis, N. obtusifolia, N. occidentalis subsp. Hersperis, N. pauciflora, N. petunioides, N. quadrivalvis, N. repanda, N. rotundifolia, N. solanifolia and N. spegazzinii. Various representative other types of plants from the Nicotiana species are described in Goodspeed, The Genus Nicotiana, (Chonica Botanica) (1954), U.S. Patent No. 4,660,577 to Sensabaugh Jr. et al., U.S. Patent No. 5,387,416 to White et al., U.S. Patent No. 7,025,066 to Lawson et al., U.S. Patent No. 7,798,153 to Lawrence Jr., and U.S. Patent No. 8,186,360 to Marshall et al., each of which is incorporated herein by reference. Descriptions of various types of tobacco, growing practices, and harvesting practices are found in Tobacco Production, Chemistry and Technology, Davis et al. (eds.) (1999), which is incorporated herein by reference.
[0127] Nicotiana species from which suitable tobacco materials can be obtained can be derived using genetic engineering or hybridization techniques (e.g., tobacco plants can be genetically engineered or hybridized to increase or decrease component production, characteristics, or attributes). See, for example, the types of genetic engineering of plants shown in U.S. Patent No. 5,539,093 to Fitzmaurice et al., U.S. Patent No. 5,668,295 to Wahab et al., U.S. Patent No. 5,705,624 to Fitzmaurice et al., U.S. Patent No. 5,844,119 to Weigl, U.S. Patent No. 6,730,832 to Dominguez et al., U.S. Patent No. 7,173,170 to Liu et al., U.S. Patent No. 7,208,659 to Colliver et al., and U.S. Patent No. 7,230,160 to Benning et al., U.S. Patent Application Publication No. 2006 / 0236434 to Conkling et al., and PCT WO2008 / 103935 to Nielsen et al. See also the types of tobacco described in U.S. Pat. No. 4,660,577 to Sensabaugh Jr. et al., U.S. Pat. No. 5,387,416 to White et al., and U.S. Pat. No. 6,730,832 to Dominguez et al., each of which is incorporated herein by reference.
[0128] Nicotiana species can be selected in some embodiments for the content of various compounds present therein. For example, plants can be selected on the basis that they produce relatively large amounts of one or more compounds that are desired to be isolated therefrom. In certain embodiments, plants of Nicotiana species (e.g., Galpao commun tobacco) are specifically cultivated for their richness in leaf surface compounds. Tobacco plants can be grown outdoors in greenhouses, growth chambers, or fields, or grown hydroponically.
[0129] Various parts or portions of a plant of the Nicotiana species can be included in the mixture as disclosed herein. For example, substantially all of the plant (e.g., the whole plant) can be harvested and used as is. Alternatively, various parts or pieces of the plant can be harvested or separated for further use after harvesting. For example, flowers, leaves, stems, stalks, roots, seeds, and various combinations thereof can be isolated for further use or processing. In some embodiments, the tobacco material includes tobacco leaves (lamina). The mixtures disclosed herein can include processed tobacco parts or pieces, dry-processed and aged tobacco in essentially natural lamina and / or stem form, tobacco extracts, extracted tobacco pulp (e.g., using water as a solvent), or mixtures of the above (e.g., a mixture in which extracted tobacco pulp is combined with granulated dry-processed and aged natural tobacco lamina).
[0130] In certain embodiments, the tobacco material comprises a solid tobacco material selected from the group consisting of lamina and stem. The tobacco used in the mixture most preferably comprises tobacco lamina, or a mixture of tobacco lamina and stem, at least a portion of which is smoked. The tobacco portions in the mixture may have a processed form, such as processed tobacco stems (e.g., cut-rolled stems, cut-rolled expanded stems, or cut-puffed stems), or volume-expanded tobacco (e.g., puffed tobacco, such as dry ice expanded tobacco (DIET)). See, for example, the tobacco expansion methods set forth in U.S. Patent No. 4,340,073 to de la Burde et al., U.S. Patent No. 5,259,403 to Guy et al., U.S. Patent No. 5,908,032 to Poindexter et al., and U.S. Patent No. 7,556,047 to Poindexter et al., all of which are incorporated by reference. Additionally, the mixture may optionally incorporate fermented tobacco. See also the types of tobacco processing techniques described in Atchley et al., PCT WO2005 / 063060, which is incorporated herein by reference.
[0131] Tobacco materials are typically used in a form that can be described as granular (i.e., shredded, crushed, granular, or powdered). There are various methods for rendering tobacco materials into comminuted or powdered form. Preferably, plant parts or fragments are comminuted, crushed, or powdered into granular form using equipment and techniques for crushing, milling, and the like. Most preferably, the plant material is in a relatively dry form during crushing or milling, using equipment such as hammer mills, cutter heads, air controlled mills, and the like. For example, tobacco parts or fragments may be crushed or milled when their moisture content is less than about 15 weight percent, or less than about 5 weight percent. Most preferably, tobacco materials are used in the form of parts or fragments having an average particle size between 1.4 millimeters and 250 microns. In some cases, the tobacco particles can be sized to pass through a screen mesh to obtain the required particle size range. If desired, air classification equipment can be used to ensure that small tobacco particles of the desired size, or range of sizes, are harvested. If desired, granulated tobacco of different sizes may be mixed together.
[0132] The manner in which tobacco is provided in a divided or powdered form can vary. Preferably, tobacco parts or pieces are comminuted, crushed, or pulverized into a powder type form, such as by using equipment and techniques for crushing or milling. Most preferably, the tobacco is in a relatively dry form during crushing or milling, such as by using equipment such as hammer mills, cutter heads, air controlled mills, and the like. For example, tobacco parts or pieces may be crushed or milled when their moisture content is less than about 15 weight percent to less than about 5 weight percent. For example, tobacco plants or portions thereof can be separated into individual parts or pieces (e.g., leaves can be removed from the stems, and / or stems and leaves can be removed from the stalks). Harvested plants or individual parts or pieces can be further subdivided into parts or pieces (e.g., leaves can be chopped, cut, comminuted, crushed, milled, or ground into parts or pieces that can be characterized as filler type pieces, granules, particulates, or fine powder). The plant or its portion can be subjected to an external force or pressure (e.g., by being pressed or rolled). When such processing conditions are performed, the plant or its portion can have a moisture content that approximates its natural moisture content (e.g., moisture content immediately after harvest), a moisture content achieved by humidifying the plant or its portion, or a moisture content that results from drying the plant or its portion. For example, powdered, comminuted, crushed or milled pieces of the plant or its portion can have a moisture content of less than about 25 weight percent, often less than about 20 weight percent, and frequently less than about 15 weight percent.
[0133] For the preparation of oral products, harvested plants of Nicotiana species are typically subjected to a curing process. The tobacco materials incorporated into the mixture for inclusion in the products as disclosed herein are appropriately cured and / or aged. A description of different types of curing processes for different types of tobacco can be found in Tobacco Production, Chemistry and Technology, Davis et al. (eds.) (1999). Examples of flue-cured tobacco techniques and conditions are found in Nestor et al., Beitrage Tabakforsch. Int., 20, 467-475 (2003) and Peele, U.S. Patent No. 6,895,974, which are incorporated herein by reference. Exemplary techniques and conditions for air-curing tobacco are described in U.S. Patent No. 7,650,892 to Groves et al., Roton et al., Beitrage Tabakforsch. Int., 21, 305-320 (2005), and Staaf et al., Beitrage Tabakforsch. Int., 21, 321-330 (2005), which are incorporated herein by reference. Certain types of tobacco may be subjected to other types of torrefaction treatments, such as fire curing or sun curing.
[0134] In certain embodiments, tobacco materials that may be employed include flue-cured or Virginia (e.g., K326), Valley, sun-cured (e.g., Indian Kurnool and Oriental tobaccos, including Katerini, Prelip, Komotini, Xanthi and Yambol tobaccos), Maryland, dark, fire and smoke cured, dark air-cured (e.g., Madole, Passanda, Cubano, Jatin and Bezuki tobaccos), light air-cured (e.g., North Wisconsin and Galpao tobaccos), Indian air-cured, Red Russian and Rustica tobaccos, as well as various other rare or specialty tobaccos and various blends of any of the foregoing tobaccos.
[0135] The tobacco material may also have a so-called "blend" form. For example, the tobacco material may include a mixture of flue-cured, valle (e.g., Malawi valle) and Oriental tobacco parts or pieces (e.g., tobacco composed of or derived from tobacco lamina or a mixture of tobacco lamina and tobacco stem). For example, a representative blend may incorporate, on a dry weight basis, about 30 to about 70 parts valle tobacco (e.g., lamina, or lamina and stem), and about 30 to about 70 parts flue-cured tobacco (e.g., stem, lamina, or lamina and stem). Other exemplary tobacco blends include, on a dry weight basis, about 75 parts flue-cured tobacco, about 15 parts ree tobacco, and about 10 parts Oriental tobacco, or about 65 parts flue-cured tobacco, about 25 parts valle, and about 10 parts Oriental tobacco, or about 65 parts flue-cured tobacco, about 10 parts valle, and about 25 parts Oriental tobacco. Another exemplary tobacco blend incorporates, on a dry weight basis, from about 20 to about 30 parts Oriental tobacco and from about 70 to about 80 parts flue-cured tobacco.
[0136] The tobacco material used in the present disclosure can be subjected to, for example, fermentation, bleaching, etc. If desired, the tobacco material can be subjected to, for example, irradiation, pasteurization, or other controlled heat treatment. Such treatment methods are detailed, for example, in U.S. Patent No. 8,061,362 to Mua et al., which is incorporated herein by reference. In certain embodiments, the tobacco material can be treated with water and an additive that can inhibit the reaction of asparagine to form acrylamide upon heating of the tobacco material (e.g., an additive selected from the group consisting of lysine, glycine, histidine, alanine, methionine, cysteine, glutamic acid, aspartic acid, proline, phenylalanine, valine, arginine, compositions incorporating divalent and trivalent cations, asparaginase, certain non-reducing sugars, certain reducing agents, phenolic compounds, certain compounds having at least one free thiol group or functional group, oxidizing agents, oxidation catalysts, natural plant extracts (e.g., rosemary extract), and combinations thereof). See, for example, the types of treatment methods described in U.S. Patent Nos. 8,434,496, 8,944,072, and 8,991,403 to Chen et al., all of which are incorporated herein by reference. In certain embodiments, this type of treatment is useful when the original tobacco material is exposed to heat in the aforementioned methods.
[0137] In some embodiments, the type of tobacco material is selected to initially be somewhat visually lighter in color than other tobacco materials (e.g., whitened or bleached). Tobacco pulp can be whitened in certain embodiments according to any means known in the art. For example, bleached tobacco materials produced by various whitening methods using various bleaching or oxidizing agents and oxidation catalysts can be used. Examples of oxidizing agents include peroxides (e.g., hydrogen peroxide), chlorites, chlorates, perchlorates, hypochlorites, ozone, ammonia, potassium permanganate, and combinations thereof. Examples of oxidation catalysts are titanium dioxide, manganese dioxide, and combinations thereof.Methods for treating tobacco with bleaching agents are described, for example, in U.S. Pat. No. 787,611 to Daniels Jr., U.S. Pat. No. 1,086,306 to Oelenheinz, U.S. Pat. No. 1,437,095 to Delling, U.S. Pat. No. 1,757,477 to Rosenhoch, U.S. Pat. No. 2,122,421 to Hawkinson, U.S. Pat. No. 2,148,147 to Baier, U.S. Pat. No. 2,170,107 to Baier, U.S. Pat. No. 2,274,649 to Baier, U.S. Pat. No. 2,770,239 to Pratz et al., U.S. Pat. No. 3,612,066 to Rosenhoch, U.S. Pat. No. 2,122,421 to Hawkinson, U.S. Pat. No. 2,148,147 to Baier, U.S. Pat. No. 2,170,107 to Baier, U.S. Pat. No. 2,274,649 to Baier, U.S. Pat. No. 2,274,649 to Pratz et al., U.S. Pat. No. 2,770,239 to Pratz, U.S. Pat. No. 2,122,066 to Rosenhoch, U.S. Pat. No. 2,122,421 to Rosenhoch, U.S. Pat. No. 2,148,147 to Baier, U.S. Pat. No. 2,170,107 to Baier, U.S. Pat. No. 2,274,649 to Rosenhoch, U.S. Pat. No. 2, No. 5, U.S. Patent No. 3,851,653 to Rosen, U.S. Patent No. 3,889,940 to Rosen, U.S. Patent No. 3,943,940 to Minami, U.S. Patent No. 3,943,945 to Rosen, U.S. Patent No. 4,143,666 to Rainer et al., U.S. Patent No. 4,194,514 to Campbell, U.S. Patent No. 4,366,823 to Rainer et al., U.S. Patent No. 4,366,824 to Rainer et al., U.S. Patent No. 4,388,933 to Schmekel et al., U.S. Patent No. 5,713,376 to Berger et al., U.S. Patent No. 4,641,667 to Schmekel et al., U.S. Patent No. 5,713,376 to Byrd et al. No. 9,339,058 to Byrd Jr. et al., U.S. Pat. No. 9,420,825 to Beeson et al., and U.S. Pat. No. 9,950,858 to Byrd Jr. et al., as well as U.S. Patent Application Publication No. 2012 / 0067361 to Bjorkholm et al., U.S. Patent Application Publication No. 2016 / 0073686 to Crooks, U.S. Patent Application Publication No. 2017 / 0020183 to Bjorkholm, U.S. Patent Application Publication No. 2017 / 0112183 to Bjorkholm, and PCT International Publication Nos. WO1996 / 031255 to Giolvas and WO2018 / 083114 to Bjorkholm, all of which are incorporated herein by reference.
[0138] In some embodiments, the whitened tobacco material can have an ISO brightness of at least about 50%, at least about 60%, at least about 65%, at least about 70%, at least about 75%, or at least about 80%. In some embodiments, the whitened tobacco material can have an ISO brightness in the range of about 50% to about 90%, about 55% to about 75%, or about 60% to about 70%. ISO brightness can be measured according to ISO 3688:1999 or ISO 2470-1:2016.
[0139] In some embodiments, whitened tobacco materials can be characterized as being lighter in color (e.g., "whiter") than untreated tobacco materials. White is often defined with reference to the Commission Internationale de l'Eclairage (CIE) chromaticity diagram. Whitened tobacco materials, in certain embodiments, can be characterized as being closer to pure white on the chromaticity diagram than untreated tobacco materials.
[0140] In various embodiments, the tobacco material can be treated to extract soluble components of the tobacco material therefrom. As used herein, "tobacco extract" refers to an isolated component of the tobacco material that is extracted from the solid tobacco pulp by a solvent that is contacted with the tobacco material in an extraction process. Various extraction techniques for tobacco materials can be used to provide tobacco extracts and tobacco solid materials. See, for example, the extraction methods described in U.S. Patent Application Publication No. 2011 / 0247640 to Beeson et al., which is incorporated herein by reference.Other example techniques for extracting tobacco components are described in U.S. Patent No. 4,144,895 to Fiore, U.S. Patent No. 4,150,677 to Osborne Jr. et al., U.S. Patent No. 4,267,847 to Reid, U.S. Patent No. 4,289,147 to Wildman et al., U.S. Patent No. 4,351,346 to Brummer et al., U.S. Patent No. 4,359,059 to Brummer et al., U.S. Patent No. 4,506,682 to Muller, U.S. Patent No. 4,589,428 to Keritsis, U.S. Patent No. 4,605,016 to Soga et al., U.S. Patent No. 4,716,911 to Poulose et al., U.S. Patent No. 4,716,911 to Niven, U.S. Patent No. 4,720,428 ... No. 4,727,889 to Jr. et al., U.S. Pat. No. 4,887,618 to Bernasek et al., U.S. Pat. No. 4,941,484 to Clapp et al., U.S. Pat. No. 4,967,771 to Fagg et al., U.S. Pat. No. 4,986,286 to Roberts et al., U.S. Pat. No. 5,005,593 to Fagg et al., U.S. Pat. No. 5,018,540 to Grubb ... White et al. No. 60,669 to Fagg, U.S. Pat. No. 5,065,775 to White et al., U.S. Pat. No. 5,074,319 to White et al., U.S. Pat. No. 5,099,862 to White et al., U.S. Pat. No. 5,121,757 to White et al., U.S. Pat. No. 5,131,414 to Fagg, U.S. Pat. No. 5,131,415 to Munoz et al., U.S. Pat. No. 5,148,819 to Fagg, U.S. Pat. No. 5,199 to Kramer, U.S. Pat. No. 7,494 to Smith et al., U.S. Pat. No. 5,230,354 to Smith et al., U.S. Pat. No. 5,234,008 to Fagg, U.S. Pat. No. 5,243,999 to Smith, U.S. Pat. No. 5,301,694 to Raymond et al., U.S. Pat. No. 5,318,050 to Gonzalez-Parra et al., U.S. Pat. No. 5,343,879 to Teague, U.S. Pat. No. 5,360,022 to Newton, U.S. Pat. No. 5,435,325 to Clapp et al., U.S. Pat. No. 5,445,169 to Brinkley et al., U.S. Pat. No. 6,131,584 to Lauterbach, U.S. Pat. No. 6,298,859 to Kierulff et al., U.S. Pat. No. 6,772,767 to Mua et al., and U.S. Pat. No. 7,337,782 to Thompson, all of which are incorporated herein by reference.
[0141] Typical content ranges of tobacco material may vary depending on the nature and type of tobacco material and the intended effect on the final mixture, but examples include ranges of up to about 30% (or up to about 20%, or up to about 10%, or up to about 5% by weight) based on the total weight of the mixture (e.g., about 0.1 to about 15% by weight). In some embodiments, the disclosed products can be characterized as being completely free or substantially free of tobacco material (other than purified nicotine as the active ingredient). For example, certain embodiments can be characterized as having less than 1% by weight, or less than 0.5% by weight, or less than 0.1% by weight, or 0% by weight of tobacco material.
[0142] <Other additives> Other additives can be included in the disclosed mixtures. For example, the mixtures can be processed, blended, compounded, combined, and / or mixed with other materials or ingredients. The additives can be artificial, obtained or derived from herbal or biological sources. Examples of further types of additives include thickening or gelling agents (e.g., fish gelatin), emulsifiers, oral care additives (e.g., thyme oil, eucalyptus oil, and zinc), preservatives (e.g., potassium sorbate, etc.), disintegration aids, or combinations thereof. See, for example, U.S. Pat. No. 9,237,769 to Mua et al., U.S. Pat. No. 7,861,728 to Holton Jr. et al., U.S. Pat. App. Pub. No. 2010 / 0291245 to Gao et al., and U.S. Pat. App. Pub. No. 2007 / 0062549 to Holton Jr. et al., each of which is incorporated herein by reference, for their representative ingredients, combinations of ingredients, relative amounts of the ingredients, and modes and methods for using the ingredients. Typical content ranges of such additional additives can vary depending on the nature and function of the additive and its intended effect on the final mixture, and include, for example, ranges up to about 10% by weight (e.g., from about 0.1 to about 5% by weight) based on the total weight of the mixture.
[0143] The aforementioned additives can be used together (e.g., as an additive blend) or separately (e.g., individual additive components can be added at different stages involved in the preparation of the final mixture). Furthermore, the aforementioned types of additives can be encapsulated so as to be provided in the final product or mixture. Exemplary encapsulated additives are described, for example, in WO 2010 / 132444 to Atchley, which has been previously incorporated by reference herein.
[0144] In some embodiments, any one or more of the filler components, tobacco materials, and overall oral products described herein can be described as particulate materials. As used herein, the term "particulate" refers to materials in the form of a plurality of individual particles, some of which may be in the form of agglomerates of a plurality of particles, where the particles have an average length to width ratio of less than 2:1, e.g., less than 1.5:1, e.g., about 1:1. In various embodiments, the particles of the particulate material can be described as being substantially spherical or granular.
[0145] The particle size of a granular material can be measured by sieve analysis. As one skilled in the art can readily appreciate, sieve analysis (also known as classification test) is a method used to measure the particle size distribution of a granular material. Typically, sieve analysis involves nested columns of sieves, preferably including screens in the form of wire mesh fabric. A pre-weighed sample can be introduced into the top or uppermost sieve of the column, which has the largest screen opening or mesh size (i.e., the largest pore size of the sieve). Each lower sieve in the column has a progressively smaller screen opening or mesh size than the sieve above. Typically, at the base of the sieve column, there is a receiver section, which collects particles with a particle size smaller than the screen opening or mesh size (the smallest screen opening or mesh size) of the bottom or lowermost sieve of the column.
[0146] In some embodiments, the column of sieves may be placed on or in a mechanical agitator. The agitator causes vibration of each sieve in the column. The mechanical agitator may be activated for a predetermined time to ensure that all particles are collected on the appropriate sieve. In some embodiments, the column of sieves is agitated for a period of time between 0.5 minutes and 10 minutes, such as between 1 minute and 10 minutes, such as between 1 minute and 5 minutes, such as about 3 minutes. Once the agitation of the sieves in the column is complete, the material collected on each sieve is weighed. The weight of each sample on each sieve can then be divided by the total weight to obtain the percentage of mass retained on each sieve. As one skilled in the art can readily appreciate, the screen opening size or mesh size for each sieve in the column used for sieve analysis may be selected based on the granularity of the sample to be analyzed or the known maximum / minimum particle size. In some embodiments, a column of sieves may be used for the sieve analysis, where the column contains 2 to 20 sieves, e.g., 5 to 15 sieves. In some embodiments, a column of sieves may be used for the sieve analysis, where the column contains 10 sieves. In some embodiments, the maximum screen opening or mesh size of the sieve used for the sieve analysis may be 1000 μm, e.g., 500 μm, e.g., 400 μm, e.g., 300 μm.
[0147] In some embodiments, any particulate material referred to herein (e.g., filler components, tobacco materials, and total oral products) can be characterized as having at least 50% by weight of particles having a particle size as measured by sieve analysis of about 1000 μm or less, such as about 500 μm or less, such as about 400 μm or less, such as about 350 μm or less, such as about 300 μm or less. In some embodiments, at least 60% by weight of the particles of any particulate material referred to herein have a particle size as measured by sieve analysis of about 1000 μm or less, such as about 500 μm or less, such as about 400 μm or less, such as about 350 μm or less, such as about 300 μm or less. In some embodiments, at least 70% by weight of the particles of any granular material referred to herein have a particle size measured by sieve analysis of about 1000 μm or less, such as about 500 μm or less, such as about 400 μm or less, such as about 350 μm or less, such as about 300 μm or less. In some embodiments, at least 80% by weight of the particles of any granular material referred to herein have a particle size measured by sieve analysis of about 1000 μm or less, such as about 500 μm or less, such as about 400 μm or less, such as about 350 μm or less, such as about 300 μm or less. In some embodiments, at least 90% by weight of the particles of any granular material referred to herein have a particle size measured by sieve analysis of about 1000 μm or less, such as about 500 μm or less, such as about 400 μm or less, such as about 350 μm or less, such as about 300 μm or less. In some embodiments, at least 95% by weight of the particles of any granular material referred to herein have a particle size as measured by sieve analysis of about 1000 μm or less, such as about 500 μm or less, such as about 400 μm or less, such as about 350 μm or less, such as about 300 μm or less. In some embodiments, at least 99% by weight of the particles of any granular material referred to herein have a particle size as measured by sieve analysis of about 1000 μm or less, such as about 500 μm or less, such as about 400 μm or less, such as about 350 μm or less, such as about 300 μm or less.In some embodiments, about 100% by weight of the particles of any particulate material referred to herein have a particle size as measured by sieve analysis of about 1000 μm or less, such as about 500 μm or less, such as about 400 μm or less, such as about 350 μm or less, for example about 300 μm or less.
[0148] In some embodiments, at least 50% by weight, such as at least 60% by weight, for example at least 70% by weight, such as at least 80% by weight, for example at least 90% by weight, for example at least 95% by weight, for example at least 99% by weight, of the particles of any particulate material referred to herein have a particle size as measured by sieve analysis of from about 0.01 μm to about 1000 μm, such as from about 0.05 μm to about 750 μm, for example from about 0.1 μm to about 500 μm, for example from about 0.25 μm to about 500 μm. In some embodiments, at least 50% by weight, such as at least 60% by weight, for example at least 70% by weight, such as at least 80% by weight, for example at least 90% by weight, for example at least 95% by weight, for example at least 99% by weight, of the particles of any particulate material referred to herein have a particle size as measured by sieve analysis of from about 10 μm to about 400 μm, such as from about 50 μm to about 350 μm, for example from about 100 μm to about 350 μm, for example from about 200 μm to about 300 μm.
[0149] <Preparation of the mixture> The manner in which the various components of the mixture are combined may vary. Thus, for example, the overall mixture of the powdered blended components and the various components may be relatively homogenous in nature. The above components, which may be in liquid or dry solid form, may be mixed in a pre-processing step prior to mixing with any remaining components of the mixture, or may simply be mixed together with all other liquid or dry components. The various components of the mixture may be contacted, combined, or mixed using any mixing technique or device known in the art. Any mixing method that brings the blended components into intimate contact may be used, such as mixing devices that feature impellers or other structures capable of agitation. Examples of mixing equipment include casing drums, conditioning cylinders or drums, liquid spraying devices, cone-type blenders, ribbon blenders, mixers available from Littleford Day, Inc. as FKM130, FKM600, FKM1200, FKM2000, and FKM3000, Plough Share-type mixer cylinders, Hobart mixers, and the like. See, for example, the types of methods described in U.S. Patent No. 4,148,325 to Solomon et al., U.S. Patent No. 6,510,855 to Korte et al., and U.S. Patent No. 6,834,654 to Williams, each of which is incorporated herein by reference. In some embodiments, the ingredients forming the mixture are prepared so that the mixture can be used in a starch molding method to form the mixture. The manner and method of blending the mixture will be clear to those skilled in the art. See, for example, the types of methods described in U.S. Patent No. 4,148,325 to Solomon et al., U.S. Patent No. 6,510,855 to Korte et al., and U.S. Patent No. 6,834,654 to Williams, U.S. Patent No. 4,725,440 to Ridgway et al., and U.S. Patent No. 6,077,524 to Bolder et al., each of which is incorporated herein by reference.
[0150] <Constructed for oral use> Provided herein are products configured for oral use. As used herein, the term "configured for oral use" means that the product is provided in such a form that, during use, saliva in the user's mouth passes one or more of the components of the mixture (e.g., flavoring agent and / or nicotine) through the user's mouth. In certain embodiments, the product is adapted to deliver an ingredient to the user through the mucous membrane in the user's mouth, and in some cases, the ingredient is an active ingredient (e.g., including but not limited to nicotine) that can be absorbed through the mucous membrane in the mouth when the product is used.
[0151] The products configured for oral use described herein may take a variety of forms, including gels, lozenges, gums, lozenges, powders, and pouches. Gels may be soft or hard. A particular product configured for oral use is in the form of a lozenge. As used herein, the term "lozenge" refers to a dissolvable oral product resulting from solidifying a liquid or gel mixture such that the final product is a somewhat hardened solid gel. The consistency of the gel is highly variable. A particular product disclosed is in the form of a solid. A particular product may exhibit one or more of the following characteristics, for example, crispy, granular, chewy, syrupy, pasty, fluffy, smooth, and / or creamy. In certain embodiments, the desired texture properties may be selected from the group consisting of adhesiveness, cohesiveness, density, dryness, friability, granularity, stickiness, hardness, weight, moisture absorption, moisture release, mouthcoating, roughness, slipperiness, smoothness, viscosity, moisture, and combinations thereof.
[0152] Products comprising the mixtures of the present disclosure may be dissolvable. The terms "dissolve", "dissolution" and "dissolvable" as used herein refer to mixtures having water-soluble components that interact with moisture in the oral cavity and go into solution, thereby causing gradual consumption of the product. According to one aspect, the dissolvable product is capable of remaining in the user's mouth for a period of time until completely dissolved. The dissolution rate may vary over a wide range, from about 1 minute or less to about 60 minutes. For example, fast-release mixtures typically dissolve and / or release the active agent in about 2 minutes or less, often about 1 minute or less (e.g., about 50 seconds or less, about 40 seconds or less, about 30 seconds or less, or about 20 seconds or less). Dissolution may occur by any means, such as melting, mechanical disintegration (e.g., chewing), enzymatic or other chemical degradation, or by disruption of interactions between the components of the mixture. In some embodiments, the product may be dissolvable, for example, as discussed in U.S. Patent Application Publication No. 2012 / 0037175 to Cantrell et al. In other embodiments, the product does not dissolve during the time the product remains in the user's mouth.
[0153] In one embodiment, the product containing the mixture of the present disclosure is in the form of a mixture disposed in a moisture-permeable container (e.g., a moisture-permeable pouch). Such moisture-permeable pouch-format mixtures are typically used by placing one pouch containing the mixture into the mouth of a human subject / user. Generally, the pouch is placed somewhere in the user's oral cavity, e.g., under the lips, in the same manner that moist snuff products are commonly used. It is preferred that the pouch is not chewed or swallowed. Exposure to saliva then causes some of the ingredients of the mixture (e.g., flavorants and / or nicotine) to pass, e.g., through the moisture-permeable pouch, providing flavor and satisfaction to the user, without the user having to spit out any portion of the mixture. After about 10 minutes to about 60 minutes, typically about 15 minutes to about 45 minutes of use / enjoyment, a significant amount of the mixture is ingested by the human subject and the pouch can be removed from the human subject's mouth for disposal.
[0154] Thus, in certain embodiments, the mixture disclosed herein and any other components described above are combined in a moisture-permeable wrapper or pouch that acts as a container for the use of the mixture and provides a pouch product configured for oral use. Certain embodiments of the disclosure are described with reference to FIG. 9 of the accompanying drawings, and these described embodiments include a snus-type product having an outer pouch and containing the mixture described herein. As will be described in more detail below, such embodiments are provided by way of example only, and the pouch product of the disclosure can contain mixtures in other forms. The mixture / configuration of such wrappers or pouches, such as the container pouch 102 in the embodiment illustrated in FIG. 9, can vary. Referring to FIG. 9, a first embodiment of a pouch product 100 is shown. The pouch product 100 includes a moisture-permeable container in the form of a pouch 102, which contains a material 104 that contains a mixture as described herein.
[0155] Suitable packets, pouches or containers of the type used in the manufacture of smokeless tobacco products are available under the trademarks CatchDry, Ettan, General, Granit, Goteborgs Rape, Grovsnus White, Metropol Kaktus, Mocca Anis, Mocca Mint, Mocca Wintergreen, Kicks, Probe, Prince, Skruf and TreAnkrare. The mixture may be packaged in a pouch in a manner that utilizes the types of ingredients used in the manufacture of conventional snus-type products. The pouch provides a liquid-permeable container of the type that is believed to be similar in properties to the mesh-like types of materials used in the construction of tea bags. The ingredients of the mixture readily diffuse through the pouch into the mouth of the user.
[0156] Non-limiting examples of suitable types of pouches are described, for example, in U.S. Pat. No. 5,167,244 to Kjerstad and U.S. Pat. No. 8,931,493 to Sebastian et al., as well as U.S. Patent Application Publication No. 2016 / 0000140 to Sebastian et al., U.S. Patent Application Publication No. 2016 / 0073689 to Sebastian et al., U.S. Patent Application Publication No. 2016 / 0157515 to Chapman et al., and U.S. Patent Application Publication No. 2016 / 0192703 to Sebastian et al., each of which is incorporated herein by reference. The pouches can be provided as individual pouches or multiple pouches (e.g., 2, 4, 5, 10, 12, 15, 20, 25 or 30 pouches) can be linked or joined (e.g., in an end-to-end manner) so that one pouch or individual portion can be easily removed for use from a one-piece strand or matrix of pouches.
[0157] As an example, the pouch is manufactured from materials in such a manner that the pouch undergoes controlled dispersion or dissolution during use by the user. Such pouch materials can have the form of mesh, sieve, perforated paper, permeable fabric, and the like. For example, a pouch material manufactured from a mesh-like form of rice paper, or perforated rice paper, can dissolve in the mouth of the user. As a result, under normal use conditions, the pouch and the mixture each disperse completely in the mouth of the user, and thus the pouch and the mixture can be ingested by the user. Other examples of pouch materials can be manufactured using water-dispersible film-forming materials (e.g., binders such as alginates, carboxymethylcellulose, xanthan gum, pullulan, and the like), and materials that combine these materials with materials such as comminuted cellulose (e.g., fine particle size wood pulp). Although the preferred pouch materials are water-dispersible or soluble, they can be designed and manufactured such that under normal use conditions, a significant amount of the mixture contents will permeate through the pouch material before the pouch loses its physical integrity. If desired, flavoring ingredients, disintegration aids, and other desired ingredients can be incorporated into or applied to the pouch material.
[0158] The amount of material contained within each product unit, e.g., pouch, may vary. In some embodiments, the weight of the mixture within each pouch is at least about 50 mg, e.g., from about 50 mg to about 1 gram, from about 100 to 800 mg, or from about 200 to about 700 mg. In some lesser embodiments, the weight of the mixture within each pouch may be from about 100 to about 300 mg. In more embodiments, the weight of the material within each pouch may be from about 300 mg to about 700 mg. If desired, other ingredients may be included within each pouch. For example, at least one flavored strip, piece, or sheet of flavored water-dispersible or water-soluble material (e.g., a breath freshening edible film-type material) may be disposed within each pouch, with or without at least one capsule. Such strips or sheets may be folded or crumpled for easy incorporation into the pouch. See, for example, the types of materials and techniques described in U.S. Patent No. 6,887,307 to Scott et al., U.S. Patent No. 6,923,981 to Leung et al., and The EFSA Journal (2004) 85, 1-32, which are incorporated herein by reference.
[0159] The pouch products described herein can be packaged in any suitable inner packaging material and / or outer container, as described, for example, in U.S. Pat. No. 7,014,039 to Henson et al., U.S. Pat. No. 7,537,110 to Kutsch et al., U.S. Pat. No. 7,584,843 to Kutsch et al., U.S. Pat. No. 8,397,945 to Gelardi et al., U.S. Pat. No. D592,956 to Thiellier, U.S. Pat. No. D594,154 to Patel et al., and U.S. Pat. No. D625,178 to Bailey et al., as well as U.S. Pat. App. Pub. No. 2008 / 0173317 to Robinson et al., U.S. Pat. App. Pub. No. 2009 / 0014343 to Clark et al., U.S. Pat. App. Pub. No. 2009 / 0014450 to Bjorkholm, U.S. Pat. App. Pub. No. 2009 / 0014450 to Bellamah et al., and U.S. Pat. App. Pub. No. 2009 / 0014450 to Bellamah et al. See also the various types of containers for smokeless type products described in U.S. Patent Application Publication Nos. 2009 / 0250360 to Gelardi et al., 2009 / 0266837 to Gelardi et al., 2009 / 0223989 to Thiellier, 2009 / 0230003 to Thiellier, 2010 / 0084424 to Gelardi, and 2010 / 0133140 to Bailey et al., 2010 / 0264157 to Bailey et al., and 2011 / 0168712 to Bailey et al., which are incorporated herein by reference.
[0160] <Storage / Retention period> The disclosed products configured for oral use can be packaged and stored in any suitable packaging in much the same way that conventional types of smokeless tobacco products are packaged and stored. For example, multiple packets or pouches can be placed in a cylindrical container. The shelf life of the agent after preparation can vary. As used herein, "shelf life" refers to the period after preparation of the disclosed product. In some embodiments, one or more of the characteristics of the product disclosed herein (e.g., retention of whiteness, lack of color change, retention of volatile flavor components) are exhibited over some or all of the shelf life. In some embodiments, the shelf life (i.e., the period after preparation) is at least 1 day. In some embodiments, the shelf life is about 1 day, about 2 days, or about 3 days to about 1 week, or about 1 week to about 2 weeks, about 2 weeks to about 1 month, about 1 month to about 2 months, about 2 months to about 3 months, about 3 months to about 4 months, or about 4 months to about 5 months. In some embodiments, the shelf life is any number of days between about 1 and about 150 days. In certain embodiments, the storage period may be greater than 5 months, such as about 6 months, about 7 months, about 8 months, about 9 months, about 10 months, about 11 months, or about 12 months.
[0161] In some embodiments, the stabilized pouch products disclosed herein have one or more of the following: a whiteness value of greater than about 40 as determined according to the Commission Internationale de l'Eclairage (CIE) model; a delta E (ΔE) value of less than about 4 in the L*a*b* color space as measured with a handheld color meter versus a control pouch product that does not contain the one or more organic acids; and a concentration of one or more flavoring agents present that is greater than the concentration of the same one or more flavoring agents present in a control pouch product that does not contain the one or more organic acids as measured by semi-quantitative gas chromatography-mass spectrometry.
[0162] <Method of stabilizing a product designed for oral use> In another aspect, there is provided a method of stabilizing a product configured for oral use as described herein. In general, the method comprises mixing a particulate filler component with water, one or more flavoring agents, and one or more organic acids or salts thereof to form a mixture, the product having a pH of less than about 7.0. In some embodiments, the mixing comprises adding one or more organic acids in an amount of about 0.1 to about 10% of the total weight of the mixture. In some embodiments, the mixing comprises adding one or more organic acids in an amount of about 0.1 to about 0.5% of the total weight of the mixture. In some embodiments, the pH of the mixture after addition is about 5.5 to about 6.5.
[0163] In some embodiments, the mixing further comprises adding one or more salts, one or more sweeteners, one or more binders, one or more humectants, one or more gums, one or more active ingredients, tobacco materials, or combinations thereof.
[0164] In some embodiments, the mixing further comprises adding about 0.001 to about 1% by weight of a nicotine component, based on the total weight of the mixture.
[0165] In some embodiments, the method further comprises enclosing the mixture in a pouch to form a pouch product, the mixture optionally being in the form of free-flowing particles.
[0166] In some embodiments, the stabilized pouch product has a whiteness value of greater than about 40 when measured at 1 day after preparation, as determined according to the Commission Internationale de l'Eclairage (CIE) model. In some embodiments, the stabilized product has a whiteness value of about 42 to about 60. In some embodiments, the product has a whiteness value (CIE model) of greater than about 45, or greater than about 50, or greater than about 55, or greater than about 60. In some embodiments, the stabilized pouch product has a whiteness value of greater than about 40 (or any other whiteness value listed above) at 2 days, 3 days, 1 week, 2 weeks, 1 month, 2 months, 3 months, 4 months, or 5 months after preparation. In some embodiments, the stabilized pouch product has a whiteness value of greater than about 40 at 6 months, 7 months, 8 months, 9 months, 10 months, 11 months, or 12 months after preparation.
[0167] In some embodiments, the stabilized pouched product has a whiteness value of greater than about 40 when measured according to the E313 Whiteness Index (ASTM Method E313) when measured at 1 day after preparation. In some embodiments, the stabilized product has an E313 whiteness value of about 42 to about 65. In some embodiments, the product has an E313 whiteness value of greater than about 45, or greater than about 50, or greater than about 55, or greater than about 60. In some embodiments, the stabilized pouched product has an E313 whiteness value of greater than about 40 (or any other E313 whiteness value described above) at 2 days, 3 days, 1 week, 2 weeks, 1 month, 2 months, 2 months, 3 months, 4 months, or 5 months after preparation. In some embodiments, the stabilized pouched product has a whiteness value of greater than about 40 at 6 months, 7 months, 8 months, 9 months, 10 months, 11 months, or 12 months after preparation.
[0168] In some embodiments, the stabilized pouch product has a delta E (ΔE) value of less than about 4 in the L*a*b* color space when measured with a handheld color meter, relative to a control pouch product that does not contain one or more organic acids, when measured at a time period of 1 day after preparation. In some embodiments, the stabilized product has a ΔE value of about 0.9 to about 3.8. In some embodiments, the product has a ΔE value of less than about 3.5, or less than about 3.0, or less than about 2.5, or less than about 2.0, or less than about 1.5, or less than about 1.0. In some embodiments, the stabilized pouch product has a ΔE value of less than about 4 (or any other ΔE value described above) at a time period of 2 days, 3 days, 1 week, 2 weeks, 1 month, 2 months, 3 months, 4 months, or 5 months after preparation. In some embodiments, the stabilized pouch product has a ΔE value of less than about 4 at a time period of 6 months, 7 months, 8 months, 9 months, 10 months, 11 months, or 12 months after preparation.
[0169] In some embodiments, the stabilized pouch product has a concentration of one or more flavoring agents present that is greater than the concentration of the same one or more flavoring agents present in a control pouch product that does not contain the one or more organic acids, as measured at a one-day period after preparation, as measured by semi-quantitative gas chromatography-mass spectrometry.
[0170] In some embodiments, the concentration is greater than the concentration of the same one or more flavoring agents present in a control pouch product 2 days, 3 days, 1 week, 2 weeks, 1 month, 2 months, 3 months, 4 months, or 5 months after preparation. In some embodiments, the concentration is greater than the concentration of the same one or more flavoring agents present in a control pouch product 6 months, 7 months, 8 months, 9 months, 10 months, 11 months, or 12 months after preparation.
[0171] In another aspect, there is provided a product adapted for oral use prepared by the methods disclosed herein.
[0172] In another aspect, a stabilized product configured for oral use is provided, the product comprising a mixture comprising one or more particulate filler components, water, one or more organic acids or salts thereof, and one or more flavoring agents, wherein the product has a pH of less than about 7.0 and the product is stabilized by the one or more organic acids or salts thereof.
[0173] Many modifications and other embodiments of the invention will come to mind to those skilled in the art to which the invention pertains having the benefit of the teachings presented above. Therefore, the invention is not to be limited to the specific embodiments disclosed, and modifications and other embodiments are intended to be included within the scope of the appended claims. Although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Examples
[0174] Aspects of the invention are more fully described by the following examples which are set forth to illustrate specific aspects of the invention and are not to be construed as limiting thereof.
[0175] <General analysis method> Methanol (MeOH) was purchased from Sigma-Aldrich (St. Louis, MO, USA). Flavor specifications were obtained from the R.J. Reynolds Flavor Laboratory.
[0176] <Determination of pH> A sample of the mixture (5.0 ± 0.1 g) was placed in a sample container. Deionized water (50 ± 1 mL) was added and the mixture was stirred with a magnetic stir bar for 15 minutes. The pH was measured with a calibrated Orion Model 3 Combination electrode and instrument.
[0177] <Quantification of ethyl vanillin content> The relative amount of ethyl vanillin in various embodiments was quantitatively evaluated using gas chromatography / mass spectrometry (GC-MS) with Single Ion Monitoring (SIM) chromatograms against a calibration curve. The instrument used for quantification was an Agilent (Wilmington, Del., USA) 6890N / 5973 GC-MS. Data analysis was performed using MassHunter Quantitative Analysis 8.07.00.
[0178] Samples were precisely weighed into scintillation vials on an analytical balance to a target weight of 0.5 grams. Each sample was then diluted with 5 mL of methanol and placed on an orbital shaker at 200 RPM for 3 hours. After shaking, each sample was filtered through a 0.45 μm PVDF filter and a 1 ml aliquot was transferred to a GC sample vial. 100 μL of vanillin internal standard (9.7 μg / ml) was added to each GC sample vial. Each sample was prepared in duplicate. Detailed parameters are shown in Table 1.
[0179] [Table 1]
[0180] <Semi-quantitative method for lime-related flavors> The relative amounts of various lime-related flavors according to certain embodiments of the present disclosure were semi-quantitatively evaluated using a gas chromatograph / mass spectrometer (GC-MS) scan. The equipment used for semi-quantitation was an Agilent (Wilmington, Delaware, USA) 7890B / 5977A GC-MS. Data analysis was performed using MassHunter Qualitative Analysis B.07.00. Detailed parameters are shown in Table 2.
[0181] Each sample was accurately weighed into a scintillation vial on an analytical balance to a target weight of 0.5 g. Each sample was then diluted with 5 mL of isopropanol (5.9 mM sodium chloride as the internal standard). μThe samples were diluted with 100 µg / mL d7-quinoline and placed on an orbital shaker at 200 RPM for 3 hours. After shaking, each sample was filtered through a 0.45 µm PVDF filter and transferred to a GC sample vial for analysis. Each sample was prepared in duplicate and analyzed by GC-MS.
[0182] The amount of the internal standard substance divided by the internal standard peak area is the conversion coefficient (compound peak area x μ g of internal standard / area of internal standard = μ Each compound was semi-quantified as 1 g of compound (100 mg / kg of compound) without considering the relative extraction factor and relative response factor.
[0183] [Table 2]
[0184] <Determination of Whiteness Value (CIE) and Delta E (ΔE)> The whiteness values of pouch products containing mixtures according to various embodiments of the present disclosure were determined according to the Commission Internationale de l'Eclairage (CIE) model, and the delta E (ΔE) values were determined with a handheld color meter in the L*a*b* color space compared to a control product (see "Precise Color Communication; Color Control from Perception to Instrumentation", Konica Minolta, 2007; http: / / konicaminolta.com / instruments / about / network, which is incorporated herein by reference).
[0185] <Determination of whiteness value (E313)> In some cases, discoloration from white was assessed by the E313 Whiteness Index according to ASTM method E313 using the formula WI=(3.388Z-3Y, where Y and Z are the CIE tristimulus values measured with a handheld meter).
[0186] [Example 1. Dependence of pH on organic acid content] Samples of pouch mixtures according to embodiments of the present disclosure including microcrystalline cellulose (mcc), water, and additional ingredients disclosed herein (salt, binder, sweetener, humectant, flavor, and 4 mg nicotine) were prepared with various amounts of citric acid and the pH of the samples was determined. The dependence of the pH of the mixture on the citric acid concentration for these embodiments is provided in Figure 1. With reference to Figure 1, amounts of citric acid from about 0.075% to about 0.35% by weight resulted in a pH of the mixture between about 8.2 and about 5.3, respectively.
[0187] [Example 2. Dependence of pH on organic acid content (ethyl vanillin flavor)] Samples of pouch mixtures according to embodiments of the present disclosure containing mcc, water, and additional ingredients disclosed herein (salt, binder, sweetener, humectant, ethyl vanillin as a flavor, and 4 mg nicotine) were prepared and the pH of the samples was determined. The dependence of the pH of the mixture on the citric acid concentration for these embodiments is provided in Table 3.
[0188] [Table 3]
[0189] [Example 3. Dependence of pH on organic acid content (containing terpenes)] Samples of pouch mixtures according to embodiments of the present disclosure, including mcc, water, and additional ingredients disclosed herein (salt, binder, sweetener, humectant, terpene-containing flavor, and 4 mg nicotine), were prepared with various amounts of citric acid and the pH of the samples was determined. The dependence of the pH of the mixture on the concentration of citric acid for these embodiments is provided in Table 4.
[0190] [Table 4]
[0191] [Example 4. Evaluation of whiteness of comparative products] Samples of comparative (control) pouch mixtures containing mcc, water, and additional ingredients disclosed herein (salt, binder, sweetener, humectant, flavor (flavor package of either ethyl vanillin, lime, or cinnamon), and 4 mg nicotine) were prepared, and each sample was evaluated for whiteness and delta E (ΔE). As shown in FIG. 2, each product exhibited time-dependent darkening (loss of whiteness). With reference to FIG. 2, a control pouch product without flavor (left) was compared to target pouch products containing ethyl vanillin, lime, and cinnamon flavors, from left to right, after 72 hours, one week, and one month, respectively. Thus, with reference to FIG. 2, it was observed that the flavors interacted with the remaining ingredients in the mixture either quickly or gradually, resulting in a visible loss of whiteness. Without wishing to be bound by theory, it is believed that an alkaline pH, such as that produced when nicotine is present in the formulation, may induce various condensation reactions of chemically reactive ingredients in the flavors, resulting in a darkening effect. Over time, the darkened material, in embodiments involving a pouch mixture, causes a staining effect on the pouch.
[0192] Example 5. Evaluation of the mechanism of whiteness loss To further explore the above hypotheses regarding pH and darkening, quantitative measurements of whiteness and color change were performed on various comparative (control) pouch products. Samples of (comparative) pouch products were prepared with and without ethyl vanillin flavoring, using a base formulation containing mcc, water, and additional ingredients disclosed herein (salt, binder, sweetener, humectant, and 4 mg nicotine), and removing either or both of nicotine and alkaline buffer (sodium bicarbonate; NaHCO3). When both nicotine and NaHCO3 were present, the pH of the mixture was 9.15. Whiteness and ΔE were evaluated for each sample. The data in Table 5 showed that in the presence of ethyl vanillin, mixtures containing basic ingredients (NaHCO3 and / or nicotine) discolored, while removal of both nicotine and NaHCO3 improved the whiteness measures relative to the base formulation.
[0193] [Table 5]
[0194] Example 6. Evaluation of the whiteness of pouch products containing ethyl vanillin with and without organic acids. Samples of pouch mixtures were prepared using a base formulation containing mcc, water, and additional ingredients disclosed herein (salt, binder, sweetener, humectant, ethyl vanillin flavoring, and nicotine (4 mg or 6 mg)). In an embodiment of the invention, citric acid (0.23% or 0.35% depending on the nicotine weight) was added to provide a pH of about 6.5, and in the comparative examples (controls), no organic acids were added. Whiteness and ΔE were evaluated for each sample. FIG. 3 shows in a photograph (top) the darkening, i.e., loss of whiteness, that occurred in a control pouch product containing ethyl vanillin as a flavoring agent in the absence of an organic acid. Referring to FIG. 3, after 72 hours, the control (top) pouch showed a brown coloration that was easily observed by the naked eye. The inventive product containing citric acid retained its initial whiteness (bottom).
[0195] Example 7. Evaluation of the whiteness of pouch products containing ethyl vanillin with various concentrations of organic acids. Samples of the pouch blend embodiments were prepared from a base formulation including mcc, water, and additional ingredients disclosed herein (salt, binder, sweetener, humectant, ethyl vanillin flavor, and 4 mg nicotine). Various concentrations of citric acid were added to each sample. The samples were evaluated for whiteness and ΔE 72 hours after preparation. Whiteness as a function of organic acid concentration is shown in FIG. 4, which is a line graph showing ΔE versus organic acid concentration for embodiments including ethyl vanillin, and the data is summarized in Table 6. Surprisingly, it was found that in certain embodiments of the present disclosure, the presence of organic acid prevents pouches containing the blend from darkening rapidly and / or gradually.
[0196] [Table 6]
[0197] Example 8. Color stability, sensory palatability, and ethyl vanillin concentration in embodiments with and without organic acids. Samples of pouch product embodiments were prepared from a control base formulation containing mcc, water, and additional ingredients disclosed herein (salt, binder, sweetener, humectant, ethyl vanillin flavor, and nicotine (4 mg)). Samples of the invention had citric acid (0.23 wt%) added to a pH of about 6.5. Each sample was evaluated for ΔE and subjective sensory preference over time. The control sample discolored quickly, while the invention embodiment containing citric acid showed no discoloration over the 145 day time course (Table 7).
[0198] [Table 7]
[0199] Ethyl vanillin was also quantified for each sample. The data in Table 7 show that the concentration of ethyl vanillin was significantly lower in the discolored control sample (95.1 μg / g ethyl vanillin) when compared to the embodiment of the invention containing citric acid, which showed no discoloration (578.1 μg / g ethyl vanillin). The loss of ethyl vanillin and darkening correlated with the results of a sensory evaluation by a panel of 14 people. The panel unanimously preferred the blend of the invention containing citric acid.
[0200] Example 9. Evaluation of the whiteness of pouch products containing terpenes with and without organic acids. Samples of the pouch product embodiments were prepared from a control base formulation containing mcc, water, and additional ingredients disclosed herein (salt, binder, sweetener, humectant, terpene-containing flavoring, and nicotine (4 mg)). Citric acid was added to the inventive sample (0.23% by weight). Whiteness and ΔE were evaluated for each sample. FIG. 5 shows in a photograph (top) the darkening, i.e., loss of whiteness, that occurred in a control pouch product containing terpene as a flavoring agent in the absence of organic acid. Referring to FIG. 5, after about one week, the control pouch (top) showed a brown coloration that was easily observed by the naked eye. The inventive embodiment containing citric acid retained its initial whiteness (bottom).
[0201] Example 10. Evaluation of whiteness of lime-flavored pouch products containing various concentrations of organic acids. Samples of the pouch product embodiments were prepared from a control base formulation containing mcc, water, and additional ingredients disclosed herein (salt, binder, sweetener, humectant, terpene-containing flavor, and nicotine (4 mg)). The inventive samples had various concentrations of added citric acid. Whiteness and ΔE were evaluated for each sample. Whiteness as a function of organic acid concentration is shown in FIG. 6, which is a line graph showing ΔE values versus organic acid concentration for these embodiments, and the data is summarized in Table 8. The data shows that the inclusion of organic acids improves the whiteness / color stability of the product over time.
[0202] [Table 8]
[0203] Example 11. Color stability, sensory palatability of lime flavored embodiments with and without organic acids. Samples of the pouch product embodiments were prepared from a control base formulation containing mcc, water, and additional ingredients disclosed herein (salt, binder, sweetener, humectant, lime flavor package with terpene component, and nicotine (4 mg)). Citric acid was added to the inventive embodiment (0.23 wt%). Each sample was evaluated for whiteness and ΔE. The results are provided in Table 9.
[0204] [Table 9]
[0205] The control samples discolored rapidly, whereas the inventive embodiment containing citric acid showed no discoloration over the 148 day time course. The darkening of the control correlated with the results of a sensory evaluation by an eight-person panel. The panel's unanimous preference was in favor of the inventive mixture containing citric acid.
[0206] Additionally, sensory testing revealed that the concentration of acid was dependent on the subjective evaluation of taste (Figures 7 and 8). With reference to Figure 7, the taste intensity for this embodiment with lime flavor increased across organic acid concentrations from 0% to 0.31%. With reference to Figure 8, the citrus flavor component of this embodiment with lime flavor increased across organic acid concentrations from 0% to 0.31%.
[0207] [Example 12. Semi-quantitative method for lime-related flavoring agents] GC-MS scans were used to identify and semi-quantify the lime-related flavor compounds in the control embodiment of Example 11 and the inventive embodiment. The data (Table 10) showed that the concentrations of lime-related flavors were not dramatically different between the two samples, however there were notable differences in the concentrations of specific flavors present in each sample, with the inventive embodiment showing higher concentrations of all terpenes analyzed at 10 days after preparation.
[0208] [Table 10]
[0209] Example 13. Evaluation of whiteness over time of pouch products containing cinnamon flavor with and without organic acids. Samples of the pouch product embodiments were prepared from a control base formulation containing mcc, water, and additional ingredients disclosed herein (salt, binder, sweetener, humectant, cinnamon flavor package containing cinnamaldehyde, and 4 mg nicotine). 0.34% citric acid was added to the inventive embodiments. Whiteness and ΔE were evaluated for each sample over time. Table 11 provides color stability data over time for these embodiments. The data demonstrates a surprising retention of whiteness in the presence of 0.34% citric acid, even after 98 days, compared to a control product with no organic acid in the mixture.
[0210] [Table 11]
Claims
1. A product adapted for oral use, comprising a mixture comprising: one or more particulate filler components; water, 0.001 to 10% by weight of a nicotine component, calculated as the free base and based on the total weight of the mixture; one or more organic acids or salts thereof, comprising 0.1 to 10 wt. % of said one or more organic acids, based on the total weight of the mixture; and one or more flavoring agents, 1. A product, wherein the product has a pH of less than 7.0, and said mixture comprises 5% or less by weight of tobacco material, excluding any nicotine components present, based on the total weight of said mixture.
2. The product of claim 1 , wherein the one or more particulate filler components comprise a cellulosic material.
3. 3. The product of claim 2, wherein the cellulosic material comprises microcrystalline cellulose.
4. The product of claim 2, wherein the one or more particulate filler components further comprise a cellulose derivative in an amount of 1% to 3% by weight of the mixture.
5. 5. The product of claim 4, wherein the cellulose derivative is hydroxypropyl cellulose.
6. 10. The product of claim 1, wherein the pH of the product is from 5.5 to 6.
5.
7. 10. The product of claim 1 comprising 0.1 to 0.5 wt. % of said one or more organic acids, based on the total weight of said mixture.
8. 10. The product of claim 1, wherein the one or more organic acids are alkyl carboxylic acids, aryl carboxylic acids, or combinations thereof.
9. 10. The product of claim 1, wherein the one or more organic acids are citric acid, malic acid, tartaric acid, octanoic acid, benzoic acid, toluic acid, salicylic acid, or combinations thereof.
10. 2. The product of claim 1, wherein the one or more organic acids is citric acid.
11. 10. The product of claim 1 comprising 10-50% of said one or more particulate filler components and 5-60% by weight water, based on the total weight of said mixture.
12. 10. The product of claim 1, wherein the mixture further comprises one or more salts, one or more sweeteners, one or more binders, one or more humectants, one or more gums, one or more active ingredients, tobacco materials, or combinations thereof.
13. 10. The product of claim 1, wherein the mixture further comprises one or more active ingredients selected from the group consisting of botanicals, stimulants, amino acids, vitamins, and cannabinoids.
14. 10. The product of claim 1, wherein the one or more flavoring agents comprise a compound having a carbon-carbon double bond, a carbon-oxygen double bond, or both.
15. 10. The product of claim 1, wherein the one or more flavoring agents comprise one or more aldehydes, ketones, esters, terpenes, terpenoids, or combinations thereof.
16. 10. The product of claim 1, wherein the one or more flavoring agents include one or more of ethyl vanillin, cinnamaldehyde, sabinene, limonene, gamma-terpinene, beta-farnesene, and citral.
17. 10. The product of claim 1, wherein the one or more flavoring agents comprises ethyl vanillin.
18. 10. The product of claim 1, wherein the mixture is enclosed in a pouch to form a pouch product, optionally wherein the mixture is in the form of free-flowing particles.
19. 1. A method for stabilizing a product configured for oral use, the stabilized product comprising a mixture comprising one or more particulate filler components, water, one or more organic acids or salts thereof in an amount of 0.1-10% by weight of the total weight of the mixture, 0.001-10% by weight of a nicotine component, calculated as the free base, based on the total weight of the mixture, and one or more flavorants, the mixture comprising 5% by weight or less of tobacco material, excluding any nicotine components present, based on the total weight of the mixture, the method comprising: mixing the one or more particulate filler components with water, the one or more flavorants, the nicotine component, and the one or more organic acids or salts thereof to form a mixture, wherein the mixture has a pH of less than 7.
0.
20. 20. The method of claim 19, wherein mixing comprises adding the one or more organic acids in an amount of 0.1 to 0.5% of the total weight of the mixture.
21. 20. The method of claim 19, wherein the pH of the product is from 5.5 to 6.
5.
22. 20. The method of claim 19, wherein the one or more organic acids are alkyl carboxylic acids, aryl carboxylic acids, or combinations thereof.
23. 20. The method of claim 19, wherein the one or more organic acids are citric acid, malic acid, tartaric acid, octanoic acid, benzoic acid, toluic acid, salicylic acid, or combinations thereof.
24. 24. The method of claim 23, wherein the one or more organic acids is citric acid.
25. 20. The method of claim 19, wherein mixing further comprises adding one or more salts, one or more sweeteners, one or more binders, one or more humectants, one or more gums, one or more active ingredients, tobacco materials, or combinations thereof.
26. 20. The method of claim 19, wherein mixing further comprises adding a cellulose derivative in an amount of 1% to 3% by weight of the mixture.
27. 27. The method of claim 26, wherein the cellulose derivative is hydroxypropyl cellulose.
28. 20. The method of claim 19, wherein said mixing further comprises adding one or more active ingredients selected from the group consisting of botanicals, stimulants, amino acids, vitamins, and cannabinoids.
29. 20. The method of claim 19, wherein the one or more flavorants comprise one or more aldehydes, ketones, esters, terpenes, terpenoids, or combinations thereof.
30. 20. The method of claim 19, wherein the one or more flavoring agents include one or more of ethyl vanillin, sabinene, limonene, gamma-terpinene, beta-farnesene, and citral.
31. 20. The method of claim 19, further comprising encapsulating the mixture in a pouch to form a pouch product, optionally wherein the mixture is in the form of free-flowing particles.
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