Buccal nicotine bag product and preparation method thereof

Abstract

The invention discloses a buccal nicotine bag product and a preparation method thereof. The buccal nicotine bag product comprises a content and an outer package, the content is powdery and comprises a nicotine source and an acidic pH regulator; the outer package is a saliva permeable pouch and is used for packaging the content, so that the pH value of the buccal nicotine pouch product in pure water or saliva is smaller than 6.0. Optimizing the pH value to a weakly acidic range (pH lt; a specific buffer system and a slow-release carrier are combined to solve the problems of oral cavity stimulation, flavor limitation and high pH dependence in the using process of an existing nicotine bag, the palatability of the nicotine bag in the using process and the nicotine release efficiency in the mouth consumption process are improved, long-acting and stable nicotine delivery is achieved by controlling release kinetics, the production cost is reduced, and the nicotine bag is suitable for large-scale popularization and application. The consumption experience is improved.

Description

Technical Field

[0001] This patent belongs to the technical field of nicotine pouch products, specifically relating to a mouth-held nicotine pouch product and its preparation method. Background Technology

[0002] With the continued advancement of global tobacco control policies and the increasing health awareness of consumers, cigarette consumption has shown a downward trend year by year, while the market demand for new nicotine alternatives, such as nicotine pouches, has experienced explosive growth. According to the latest comprehensive research report on the global nicotine pouch market, the global nicotine pouch market size may reach US$23.6 billion by 2030, with a compound annual growth rate of 35.8% from 2024 to 2030. With the continuous development of market trade and the expansion of the new tobacco products market, the production and sales of nicotine pouches are gradually showing a global trend. More and more international tobacco companies are beginning to establish a global presence in the nicotine pouch market, driving the globalization of nicotine pouch production.

[0003] Nicotine pouches, as a smokeless nicotine delivery system, have rapidly emerged in the market as an alternative to traditional tobacco products in recent years. These products do not require combustion or inhalation of smoke; instead, a small pouch containing nicotine is placed between the gums and lips, allowing for direct absorption of nicotine through the oral mucosa. This avoids harmful substances such as tar and carbon monoxide produced by tobacco combustion. The process is smokeless and ash-free, allowing for discreet use in smoke-free areas and eliminating secondhand smoke, thus attracting increasing attention from consumers. However, existing nicotine pouch technology still has significant shortcomings in pH control and user experience.

[0004] Traditional nicotine pouches typically use alkaline formulations (pH ≥ 7) to promote the release of free nicotine base, thereby improving absorption efficiency through the oral mucosa. For example, US Patent Publication No. US9907748B2 uses ion exchange resin to bind nicotine and relies on carbonate buffers to maintain the pH above 8.0. Separation of the buffer from the nicotine leads to delayed nicotine release, and the highly alkaline environment causes oral mucosal irritation, manifesting as a burning sensation, gum damage, and discomfort, especially pronounced in female users. Furthermore, clinical studies have shown that products with a pH above 8.0 significantly increase the rate of nicotine absorption, potentially exacerbating addiction and triggering physiological responses such as increased heart rate and blood pressure. Chinese Patent Publication No. CN116268530A discloses a nicotine lozenge containing a pH-adjusting agent and its preparation method. This method uses microencapsulation technology to encapsulate a pH-adjusting agent with γ-cyclodextrin, allowing for slow release of the pH-adjusting agent to regulate the pH value. The patent document with publication number WO2018 / 233795 uses tobacco extract as the nicotine source. Although it adjusts the taste with sugar alcohols, it does not effectively solve the problem of alkaline irritation. In addition, although international standards such as ISO 21109:2025 specify methods for pH value determination, they do not provide guidance on acidic formulations, making it difficult for existing products to achieve a balance between reducing irritation and maintaining absorption efficiency.

[0005] Therefore, there is an urgent need to develop a nicotine pouch product that optimizes the pH value of the nicotine pouch to a slightly acidic range (pH<6.0) to achieve efficient nicotine release. This aims to solve the problems of oral irritation, limited flavor, and strong pH dependence of existing nicotine pouches during use, improve the palatability of nicotine pouches during use, increase the nicotine release efficiency during oral consumption, achieve long-term and stable nicotine delivery by controlling release kinetics, reduce production costs, and enhance the consumer experience. Summary of the Invention

[0006] The purpose of this patent is to provide a nicotine pouch product and its preparation method. By optimizing the pH value to a slightly acidic range (pH<6.0), and combining a specific buffer system and a slow-release carrier, the patent aims to solve the problems of oral irritation, limited flavor, and strong pH dependence of existing nicotine pouches during use. This will improve the palatability of the nicotine pouch during use, increase the nicotine release efficiency during oral consumption, achieve long-term and stable nicotine delivery by controlling release kinetics, reduce production costs, and enhance the consumer experience.

[0007] To solve the above-mentioned technical problems, this patent adopts the following technical solution:

[0008] A nicotine pouch product for oral use includes contents and an outer packaging; the contents are in powder form and include a nicotine source and an acidic pH adjuster; the outer packaging is a saliva-permeable pouch for sealing the contents so that the pH value of the nicotine pouch product in pure water or saliva is <6.0.

[0009] Furthermore, the amount of acidic pH adjuster added is 2.0~3.0%, 3.0~5.0%, 5.0~7.0%, or 7.0~9.0%; the acidic pH adjuster includes one or more combinations of organic acids, organic acid salts, or inorganic acid salts.

[0010] Alternatively, pH adjusters can be encapsulated with polymers, including gelatin, resin, cyclodextrin, and starch.

[0011] Furthermore, organic acids include one or more combinations of citric acid, malic acid, lactic acid, acetic acid, tartaric acid, gluconic acid, or fumaric acid.

[0012] Furthermore, organic acid salts include one or more combinations of alkali metal or ammonium citrates, malates, lactates, tartrates, gluconates, or fumarates.

[0013] Furthermore, inorganic acid salts include one or more combinations of alkali metal or ammonium carbonates, monohydrogen phosphates, dihydrogen phosphates, trihydrogen phosphates, or bicarbonates.

[0014] Furthermore, the amount of nicotine source added is 1.0~2.0%, 2.0~3.0% or 3.0~4.0%, and the nicotine source includes one or more combinations of free nicotine salts or elemental nicotine.

[0015] Furthermore, free nicotine salts include one or more combinations of nicotine hydrochloride, nicotine dihydrochloride, nicotine citrate, nicotine monotartrate, nicotine hydrogen tartrate, nicotine hydrogen tartrate dihydrate, nicotine sulfate, nicotine resinate, and nicotine salicylate.

[0016] The nicotine source may be chosen to be soluble in water or in an organic solvent, including one or more of glycerol, ethyl acetate, alcohol, triglycerides, diglycerides, and monoglycerides.

[0017] Furthermore, the contents also include fillers with a water content of ≤7.0% and particle sizes of 15~30μm, 30~50μm, 50~80μm, 80~120μm or 120~200μm.

[0018] Furthermore, the filler is a porous matrix, which is plant fiber or cellulose derivative.

[0019] Furthermore, cellulose derivatives include one or more combinations of hydrolyzed cellulose, cellulose ethers, cellulose esters, or cellulose ether esters.

[0020] Furthermore, hydrolyzed cellulose includes microcrystalline cellulose.

[0021] Furthermore, cellulose esters include one or more combinations of cellulose nitrates, cellulose acetates, cellulose acetate butyrates, or cellulose xanthates.

[0022] Furthermore, cellulose ethers include one or more combinations of methylcellulose, carboxymethylcellulose, ethylcellulose, hydroxyethylcellulose, cyanoethylcellulose, hydroxypropylcellulose, or hydroxypropylmethylcellulose.

[0023] Furthermore, the contents also include excipients, sweeteners, and flavorings.

[0024] Furthermore, the amount of excipient added is 0.1~1.0%, 1.0~2.0%, or 2.0~3.0%; the excipient includes one or more combinations of silicon dioxide, calcium silicate, calcium stearate, magnesium stearate, sodium alginate, and sodium carboxymethyl cellulose.

[0025] Furthermore, the amount of sweetener added is 0.5~2.0%, 2.0~5.0%, or 5.0~10.0%; the particle size of the sweetener is 50~80 μm, 80~120 μm, 120~180 μm, or 180~250 μm.

[0026] Furthermore, the amount of added flavorings and fragrances is 2.0~4.0%, 4.0~7.0%, or 7.0~10.0%.

[0027] Furthermore, the filling amount of the nicotine pouch product is 100~300 mg, 300~500 mg, 500~800 mg, 800~1200 mg or 1200~1500 mg; the nicotine content in the contents is 0.1~1.0 mg, 1.0~3.0 mg, 3.0~5.0 mg, 5.0~8.0 mg or 8.0~15.0 mg.

[0028] Another aspect of this patent provides a method for preparing a nicotine sachet product, comprising the following steps:

[0029] Step A: Mix the filler and sweetener to obtain a premix; add nicotine source and excipient to the premix, mix evenly to obtain a solid mixture;

[0030] Step B: Add an acidic pH adjuster and flavoring to the solid mixture, mix well, and then sieve to obtain the contents;

[0031] Step C: Fill the outer packaging with the contents, seal the edges and sterilize with ultraviolet light to obtain the oral nicotine pouch product.

[0032] Furthermore, in step A, the mass ratio of filler to sweetener is (3.0~10.0):1.

[0033] Furthermore, in step B, an acidic pH adjuster is added to the solid mixture via spraying.

[0034] The acidic pH adjuster, of any choice, is encapsulated in a polymer.

[0035] Furthermore, the cumulative nicotine release rate of the oral nicotine pouch product is >81% within the oral cavity from 0 to 35 minutes.

[0036] Furthermore, the water content in oral nicotine pouch products is 5-10%, 10-20%, 20-30%, or 30-50%.

[0037] Furthermore, the sweetener includes a first sweetener and a second sweetener, used to reduce oral irritation; the first sweetener is in powder form, and the particle size D of the first sweetener powder is... 50 The particle size is 50~100 μm; the second sweetener is granular, and the particle size D of the second sweetener is... 50 The particle size is 150~250 μm; the first sweetener has a small particle size and a fast dissolution rate, while the second sweetener has a large and coarse particle size and a slow dissolution rate, and is used to continuously stimulate the secretion of saliva in the breath.

[0038] Furthermore, both the first and second sweeteners can be selected from one or more combinations of sucrose, saccharin, sucralose, glucose, maltose, corn syrup, cyclamate, aspartame, acesulfame potassium, xylitol, mannose, salts of acesulfame (e.g., potassium butyrate), alitame, cyclohexanesulfonic acid and its salts, glycyrrhizin, dihydrochalcone, kiwifruit protein, indigofera protein, and steviol glycosides. It is understood that the first and second sweeteners may have different particle sizes, but they can be the same type of sweetener or different types of sweeteners.

[0039] Non-exhaustive examples of suitable flavorings in embodiments of the invention include coconut, coffee, chocolate, vanilla, citrus fruits (e.g., grapefruit, orange, lime, bergamot, or lemon), menthol, licorice, caramel, honey, peanut, walnut, cashew, hazelnut, almond, pineapple, strawberry, raspberry, tropical fruits, cherry, cinnamon, cumin, peppermint, deer antler, spearmint, eucalyptus, mint, and fruit flavorings (e.g., flavorings from apple, pear, peach, strawberry, apricot, raspberry, cherry, pineapple, lemongrass, lime, chili (capsaicin), citrus, tobacco flavor, bergamot, and plum). Preferably, the flavorings also comprise essential oils, including one or more combinations of peppermint, spearmint, menthol, eucalyptus, clove oil, laurel oil, fennel, thyme, cedarwood oil, nutmeg, and oils from the aforementioned fruits.

[0040] As used in this patent, a "nicotine pouch" generally refers to a small fibrous pouch that absorbs nicotine through the lining of the mouth, and its main components are nicotine powder or nicotine salts. They are typically placed between the gums and the upper lip, and the nicotine is absorbed by the body through the oral mucosa.

[0041] As used in this patent, "nicotine" (also known as nicotine) has the chemical formula C. 10 H 14 N2 is a pyridine alkaloid. In this article, the terms "nicotine" and "nicotine alkaloid" are used interchangeably.

[0042] As used in this patent, "particle size" generally refers to the diameter of the particle, and particle size is usually expressed using particle size. "D" 50 "This typically refers to the particle size at which the cumulative force distribution percentage of a sample reaches 50%. Physically, it means that 50% of the particles are larger than this size, and 50% are smaller than it. D" 50 Also called median diameter or median particle size, it is usually used to represent the average particle size.

[0043] This patent provides a nicotine pouch product and its preparation method, which optimizes the pH value of the nicotine pouch product to a weakly acidic range (pH<6.0) to achieve efficient nicotine release. This aims to solve the problems of oral irritation, limited flavor, and strong pH dependence of existing nicotine pouches during use, improve the palatability of nicotine pouches during use, increase the nicotine release efficiency during oral consumption, achieve long-term stable nicotine delivery by controlling release kinetics, reduce production costs, and enhance the consumer experience. Attached Figure Description

[0044] The above content of this patent and the following detailed embodiments will be better understood when read in conjunction with the accompanying drawings. It should be noted that the drawings are merely examples of the claimed technical solution.

[0045] Figure 1 This is a flowchart illustrating the preparation process of the oral nicotine pouch product in this patent. Detailed Implementation

[0046] The following detailed description of the features and advantages of this application is sufficient to enable any person skilled in the art to understand the technical content of this application and implement it accordingly. Based on the specification, claims and drawings disclosed in this specification, those skilled in the art can easily understand the related objectives and advantages of this application.

[0047] In this specification and claims, several terms will be used, and unless otherwise indicated, these terms will be defined to have the following meanings:

[0048] All figures used to represent component amounts, properties (e.g., weight-average molecular weight), reaction conditions, etc., should be considered to be modified in all cases by the terms "within the unavoidable margin of error" or "approximately". Therefore, the numerical values ​​presented herein are approximate and may vary depending on the desired properties sought to be obtained by this patent. The principle of equivalents, which is applied to a minimum and not intended to limit the scope of the claims, should be applied, for example, each value should be interpreted at least according to the reported significant digits and by applying conventional rounding techniques.

[0049] All other terms used herein for special definition are intended to have the general meaning understood by one of ordinary skill in the art, in particular meaning that one of ordinary skill in the art, upon reading the claims, specification and drawings of this patent, can directly and without doubt determine how the technical solution of this patent can be implemented.

[0050] Even if there are incomplete descriptions, omissions, or ambiguities in the grammar, words, punctuation, graphics, symbols, etc. of the claims, specification, and drawings of this patent, a person skilled in the art can still arrive at the only correct understanding by reading the claims, specification, and drawings as a whole without extensive reasoning or experimentation, and effectively exclude various incorrect interpretations that are not aimed at achieving the purpose of this patent.

[0051] The "range" disclosed herein is defined by a lower limit and an upper limit. A given range is defined by selecting a lower limit and an upper limit, which define the boundaries of a particular range. Ranges defined in this way can include or exclude endpoints and can be arbitrarily combined; that is, any lower limit can be combined with any upper limit to form a range. For example, if ranges of 60-120 and 80-110 are listed for a specific parameter, it is expected that ranges of 60-110 and 80-120 are also expected. Furthermore, if minimum range values ​​of 1 and 2 are listed, and if maximum range values ​​of 3, 4, and 5 are listed, then the following ranges are all expected: 1-3, 1-4, 1-5, 2-3, 2-4, and 2-5. In this application, unless otherwise stated, the numerical range "ab" represents a shortened representation of any combination of real numbers between a and b, where a and b are real numbers. For example, the numerical range "0-5" indicates that all real numbers between "0-5" have been listed in this article; "0-5" is simply a shortened representation of these numerical combinations. Furthermore, when a parameter is stated as an integer ≥2, it is equivalent to disclosing that the parameter is, for example, an integer such as 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc.

[0052] Unless otherwise specified, all embodiments and preferred embodiments mentioned herein can be combined to form new technical solutions.

[0053] Unless otherwise specified, all the technical features and preferred features mentioned herein can be combined to form new technical solutions.

[0054] Unless otherwise specified, all steps mentioned herein may be performed sequentially or randomly, but are preferably performed sequentially. For example, the method includes steps (a) and (b), indicating that the method may include steps (a) and (b) performed sequentially, or it may include steps (b) and (a) performed sequentially. For example, the mention that the method may also include step (c) indicates that step (c) may be added to the method in any order; for example, the method may include steps (a), (b), and (c), or it may include steps (a), (c), and (b), or it may include steps (c), (a), and (b), etc.

[0055] Unless otherwise specified, the terms "comprising" and "including" as used herein can be open-ended or closed-ended. For example, "comprising" and "including" may mean that other components not listed may also be included, or that only the listed components may be included.

[0056] In the description of this article, it should be noted that, unless otherwise stated, "above" and "below" include the number itself, and "several" in "one or more" means two or more.

[0057] In this description, unless otherwise stated, the term "or" is inclusive. For example, the phrase "A or B" means "A, B, or both A and B". More specifically, the condition "A or B" is satisfied by any of the following conditions: A is true (or exists) and B is false (or does not exist); A is false (or does not exist) and B is true (or exists); or both A and B are true (or exist).

[0058] Unless otherwise specified, percentages (%) in this document refer to percentages by mass relative to the composition.

[0059] Unless otherwise stated herein, the sum of the contents of the components in the composition is 100%.

[0060] In this document, unless otherwise stated, “combination of” means a multi-component mixture of the elements, such as two, three, four, and up to the maximum possible multi-component mixture.

[0061] Unless otherwise specified, the term "a" as used in this specification means "at least one".

[0062] The terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this invention, "a plurality of" means at least two, such as two, three, etc., unless otherwise explicitly specified.

[0063] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.

[0064] To make the objectives, technical solutions, and advantages of the present invention clearer, the embodiments of the present invention will be further described in detail below with reference to the accompanying drawings. Unless otherwise specified, the experimental methods described in the embodiments of the present invention are conventional methods, and the materials and reagents used in the following embodiments are commercially available unless otherwise specified.

[0065] like Figure 1 As shown, this patent provides a nicotine-filled pouch product and its preparation method, with the specific steps as follows:

[0066] (1) The porous matrix and sweetener are mixed evenly at a mass ratio of (3.0~5.0):1 to obtain the first mixture;

[0067] The porous matrix is ​​composed of plant fibers or cellulose derivatives. Plant fibers include wheat fiber, corn fiber, sunflower fiber, or rice fiber; cellulose derivatives include one or more combinations of hydrolyzed cellulose, cellulose ethers, cellulose esters, or cellulose ether esters; hydrolyzed cellulose includes microcrystalline cellulose; cellulose esters include cellulose nitrates, cellulose acetates, cellulose acetate butyrate, or cellulose xanthates; cellulose ethers include methylcellulose, carboxymethylcellulose, ethylcellulose, hydroxyethylcellulose, cyanoethylcellulose, hydroxypropylcellulose, or hydroxypropyl methylcellulose. The powder particle size D of the porous matrix is... 50 The size is 15~200 μm, and the water content is ≤7.0%.

[0068] Sweeteners include a primary sweetener and a secondary sweetener, used to reduce oral irritation; the primary sweetener is in powder form, and the particle size D of the primary sweetener powder is... 50 The particle size is 50~100 μm; the second sweetener is granular, and the particle size D of the second sweetener is... 50 The particle size is 150~250 μm; the first sweetener has a small particle size and a fast dissolution rate, while the second sweetener has a large and coarse particle size and a slow dissolution rate, and is used to continuously stimulate the secretion of saliva in the breath.

[0069] Both the first and second sweeteners can be selected from one or more combinations of sucrose, saccharin, sucralose, glucose, maltose, corn syrup, cyclamate, aspartame, acesulfame potassium, xylitol, mannose, salts of acesulfame (e.g., potassium butysulfame), alitame, cyclohexanesulfonic acid and its salts, glycyrrhizin, dihydrochalcone, kiwifruit protein, indigofera protein, and steviol glycosides. It is understood that the first and second sweeteners may have different particle sizes, but they can be the same type of sweetener or different types of sweeteners.

[0070] (2) Add nicotine source to the first mixture. The mass ratio of the amount of nicotine source added to the amount of the first mixture is 1:(15~60). After mixing evenly, the second mixture is obtained.

[0071] The nicotine source is one or a combination of two of the following: free nicotine salts or elemental nicotine. Free nicotine salts include one or a combination of nicotine hydrochloride, nicotine dihydrochloride, nicotine citrate, nicotine monotartrate, nicotine hydrogen tartrate, nicotine hydrogen tartrate dihydrate, nicotine sulfate, nicotine resinate, or nicotine salicylate. The nicotine source is soluble in water or in organic solvents, including one or more of glycerol, ethyl acetate, alcohols, triglycerides, diglycerides, and monoglycerides.

[0072] (3) Add excipients to the second mixture, the amount of excipients added is 3.0% to 6.0% of the mass percentage of the amount of the second mixture added, and mix evenly to obtain the third mixture;

[0073] The excipients include one or more of silicon dioxide, calcium silicate, calcium stearate, magnesium stearate, sodium alginate, and sodium carboxymethyl cellulose.

[0074] (4) Mix the pH adjuster with pure water at a ratio of 1:(3.0~12.0) to obtain a pH adjuster aqueous solution;

[0075] The pH adjuster is an acidic adjuster, including single organic acids, combinations of organic acids and organic acid salts, combinations of organic acids and inorganic acid salts, or combinations of organic acids and sweeteners. Organic acids include citric acid, malic acid, lactic acid, acetic acid, tartaric acid, gluconic acid, and fumaric acid; organic acid salts include alkali metal or ammonium citrates, malates, lactates, tartrates, glucosides, and fumarates; inorganic acid salts include alkali metal or ammonium carbonates, monohydrogen phosphates, dihydrogen phosphates, trihydrogen phosphates, and bicarbonates; sweeteners include steviol glycosides, mogrosides, erythritol, sucralose, acesulfame potassium, sodium saccharin, neotame, alitane, and one or more mixtures of cyclamate. pH adjusters can also be encapsulated with polymers, including gelatin, resins, cyclodextrin, and starch.

[0076] (5) The pH adjuster aqueous solution prepared in step (4) is sprayed evenly into the third mixture being stirred in step (3) by spraying. The mass of the pH adjuster aqueous solution added is 20-30% of the mass of the third mixture added, to obtain the fourth mixture.

[0077] (6) Add flavorings and fragrances to the fourth mixture. The amount of flavorings and fragrances added is 3.0 to 6.0% of the amount of the fourth mixture, to obtain the fifth mixture.

[0078] The flavorings and fragrances are a non-exhaustive list, including coconut, coffee, chocolate, vanilla, citrus fruits (e.g., grapefruit, orange, lime, bergamot, or lemon), menthol, licorice, caramel, honey, peanut, walnut, cashew, hazelnut, almond, pineapple, strawberry, raspberry, tropical fruits, cherry, cinnamon, cumin, peppermint, deer antler, spearmint, eucalyptus, mint, and fruit flavorings (e.g., flavorings from apple, pear, peach, strawberry, apricot, raspberry, cherry, pineapple, lemongrass, lime, chili (capsaicin), citrus, tobacco flavor, bergamot, and plum). Preferably, the flavorings and fragrances also include essential oils, including any one or more combinations of peppermint, spearmint, menthol, eucalyptus, clove oil, laurel oil, fennel, thyme, cedarwood oil, nutmeg, and oils from the aforementioned fruits.

[0079] (7) The fifth mixture obtained in step (6) above is sieved so that the mesh size of the fifth mixture is 80~300 mesh, and a powder mixture is obtained. The powder mixture is collected as the contents.

[0080] (8) The contents prepared in step (7) are filled into saliva-permeable pouches using a packaging machine. The contents of each saliva-permeable pouch are 100-1500 mg, of which the salt and alkali content is 0.1-15.0 mg. After sealing and ultraviolet sterilization, the oral nicotine pouch product is obtained.

[0081] The saliva-permeable sachets are made of medical-grade nonwoven fabric, lyocell, modal, or tencel, and the quantitative amount of the saliva-permeable sachets is 25~35 g / m³. 2 .

[0082] Example 1

[0083] (1) Weigh 192 g of microcrystalline cellulose, 7 g of erythritol and 40.8 g of maltitol respectively, and place them in a ribbon conical mixer (commercially available) for stirring to obtain the first mixture;

[0084] (2) Add 9.6 g of nicotine tartrate to the first mixture and continue stirring to obtain the second mixture;

[0085] (3) Add 10.5 g of silicon dioxide to the second mixture and stir continuously to obtain the third mixture;

[0086] (4) Weigh 8.4 g of citric acid and dissolve it in 52.5 g of water. After mixing evenly, a pH adjusting agent aqueous solution is obtained.

[0087] (5) The pH adjuster aqueous solution prepared in step (4) is sprayed evenly onto the third mixture being stirred in step (3) to obtain the fourth mixture;

[0088] (6) Add 14 g of peppermint extract to the fourth mixture to obtain the fifth mixture;

[0089] (7) The fifth mixture is sieved so that the mesh size of the fifth mixture is 100 mesh to obtain a powder mixture, which is collected as the contents;

[0090] (8) The contents prepared in step (7) are filled into non-woven fabric bags using a packaging machine. The contents of each non-woven fabric bag are 350 mg. After sealing and ultraviolet sterilization, the oral nicotine bag product is obtained and marked as P1.

[0091] Example 2

[0092] (1) Weigh 267 g of microcrystalline cellulose, 20 g of xylitol and 54 g of maltitol respectively, and place them in a ribbon conical mixer (commercially available) for stirring to obtain the first mixture;

[0093] (2) Add 12.8 g of nicotine citrate to the first mixture and continue stirring to obtain the second mixture;

[0094] (3) Add 18 g of silicon dioxide to the second mixture and stir continuously to obtain the third mixture;

[0095] (4) Weigh 12 g of citric acid and dissolve it in 75 g of water. After mixing evenly, a pH adjusting agent aqueous solution is obtained.

[0096] (5) The pH adjuster aqueous solution prepared in step (4) is sprayed evenly onto the third mixture being stirred in step (3) to obtain the fourth mixture;

[0097] (6) Add 20 g of lemon flavoring to the fourth mixture to obtain the fifth mixture;

[0098] (7) The fifth mixture is sieved so that the mesh size of the fifth mixture is 100 mesh to obtain a powder mixture, which is collected as the contents;

[0099] (8) The contents prepared in step (7) are filled into non-woven fabric bags using a packaging machine. The contents of each non-woven fabric bag are 500 mg. After sealing and ultraviolet sterilization, the oral nicotine bag product is obtained and marked as P2.

[0100] Example 3

[0101] (1) Weigh 275g of microcrystalline cellulose, 20g of mannitol and 59g of erythritol respectively, and place them in a ribbon conical mixer (commercially available) for stirring to obtain the first mixture;

[0102] (2) Add 6.4 g of nicotine malate to the first mixture and continue stirring to obtain the second mixture;

[0103] (3) Add 15 g of calcium silicate to the second mixture and stir continuously to obtain the third mixture;

[0104] (4) Weigh 19 g of malic acid and dissolve it in 75 g of water. After mixing evenly, a pH adjusting agent aqueous solution is obtained.

[0105] (5) The pH adjuster aqueous solution prepared in step (4) is sprayed evenly onto the third mixture being stirred in step (3) to obtain the fourth mixture;

[0106] (6) Add 20 g of peppermint essence to the fourth mixture to obtain the fifth mixture;

[0107] (7) The fifth mixture is sieved so that the mesh size of the fifth mixture is 150 mesh, and a powder mixture is obtained. The powder mixture is collected as the contents.

[0108] (8) The contents prepared in step (7) are filled into non-woven fabric bags using a packaging machine. The contents of each non-woven fabric bag are 500 mg. After sealing and ultraviolet sterilization, the oral nicotine bag product is obtained and marked as P3.

[0109] Example 4

[0110] (1) Weigh 243 g of microcrystalline cellulose, 19 g of sucralose and 59 g of maltitol respectively, and put them into a ribbon conical mixer (commercially available) for stirring to obtain the first mixture;

[0111] (2) Add 19.2 g of nicotine hydrochloride to the first mixture and continue stirring to obtain the second mixture;

[0112] (3) Add 15 g of calcium stearate to the second mixture and continue stirring to obtain the third mixture;

[0113] (4) Weigh 7 g of tartaric acid and dissolve it in 75 g of water. After mixing evenly, a pH adjusting agent aqueous solution is obtained.

[0114] (5) The pH adjuster aqueous solution prepared in step (4) is sprayed evenly onto the third mixture being stirred in step (3) to obtain the fourth mixture;

[0115] (6) Add 35 g of coffee flavoring to the fourth mixture to obtain the fifth mixture;

[0116] (7) The fifth mixture is sieved so that the mesh size of the fifth mixture is 200 mesh, and a powder mixture is obtained. The powder mixture is collected as the contents.

[0117] (8) The contents prepared in step (7) are filled into non-woven fabric bags using a packaging machine. The contents of each non-woven fabric bag are 500 mg. After sealing and ultraviolet sterilization, the oral nicotine bag product is obtained and marked as P4.

[0118] Example 5

[0119] (1) Weigh 520 g of microcrystalline cellulose, 47 g of sucrose and 110 g of acesulfame potassium respectively, and put them into a ribbon cone mixer (commercially available) for mixing to obtain the first mixture;

[0120] (2) Add 12.8 g of nicotine tartrate to the first mixture and continue stirring to obtain the second mixture;

[0121] (3) Add 25 g of silicon dioxide to the second mixture and stir continuously to obtain the third mixture;

[0122] (4) Weigh 44 g of citric acid and dissolve it in 170 g of water. After mixing evenly, a pH adjusting agent aqueous solution is obtained.

[0123] (5) The pH adjuster aqueous solution prepared in step (4) is sprayed evenly onto the third mixture being stirred in step (3) to obtain the fourth mixture;

[0124] (6) Add 50 g of orange flavoring to the fourth mixture to obtain the fifth mixture;

[0125] (7) The fifth mixture is sieved so that the mesh size of the fifth mixture is 200 mesh, and a powder mixture is obtained. The powder mixture is collected as the contents.

[0126] (8) The contents prepared in step (7) are filled into non-woven fabric bags using a packaging machine. The contents of each non-woven fabric bag are 1000 mg. After sealing and ultraviolet sterilization, the oral nicotine bag product is obtained and marked as P5.

[0127] Comparative Example 1

[0128] Compared with Example 2, the difference is that this comparative example uses an alkaline pH adjuster and sodium carbonate and sodium bicarbonate as additives to prepare a nicotine-containing pouch product, labeled as A1.

[0129] Comparative Example 2

[0130] Compared with Example 2, the difference is that this comparative example uses an alkaline pH adjuster and sodium carbonate and sodium bicarbonate as additives to prepare a nicotine-containing pouch product, labeled as A2.

[0131] Comparative Example 3

[0132] Compared with Example 3, the difference is that this comparative example uses an alkaline pH adjuster and sodium carbonate and sodium bicarbonate as additives to prepare a nicotine-containing pouch product, labeled as A3.

[0133] Comparative Example 4

[0134] Compared with Example 3, the difference is that this comparative example uses an alkaline pH adjuster and sodium carbonate and sodium bicarbonate as additives to prepare a nicotine-containing pouch product, labeled A4.

[0135] Test Example 1: pH value determination of nicotine leaching

[0136] The pH value of nicotine leaching was measured for the oral nicotine pouch products (P1-P5) in Examples 1-5 and the oral nicotine pouch products (A1-A4) in Comparative Examples 1-4.

[0137] The specific testing method is as follows: Take 30 beakers with a capacity of 100 mL, add 10 mL of pure water to each beaker, set up 3 products without oral nicotine pouches as blank controls, place oral nicotine pouch products P1~P5 and A1~A4 in beakers respectively, set up 3 technical replicates for each oral nicotine pouch product, calibrate the nicotine dissolution time to 10 min, and then use a pH meter to measure the pH value after nicotine dissolution and take the average value.

[0138] The results are shown in Table 1: The pH values ​​of the oral nicotine pouch products (P1~P5) prepared by the methods provided in Examples 1~5 after contact with pure water were all significantly lower than the pH values ​​of the oral nicotine pouch products (A1~A4) in Comparative Examples 1~4 after contact with pure water.

[0139] Table 1. Statistical table of pH values ​​after nicotine dissolution in nicotine pouch products.

[0140] Test Example 2

[0141] Nicotine release experiments were conducted on oral nicotine pouch product P2 (containing 500 mg of contents per pouch, of which nicotine content is 6 mg per pouch) prepared in Example 2, and oral nicotine pouch products A1 and A2 of Comparative Example 1, which have the same contents and nicotine content.

[0142] The specific method is as follows: 100 mL of simulated artificial saliva with a pH of 6.8 is placed in each beaker and maintained at 37.0±0.1℃. A nicotine sachet with the same nicotine content is placed in each beaker, and the mixture is stirred at 100 rpm. A precise sample of 2 mL is taken every minute until 10 minutes have elapsed. After 10 minutes, a sample is taken every 10 minutes, with 2 mL of simulated artificial saliva added after each sample (to simulate the cumulative nicotine release in the oral cavity, artificial saliva needs to be added after each sample as saliva is continuously secreted). The 2 mL solution is then diluted to 10 mL with simulated artificial saliva. The nicotine content is detected using HPLC, and the relative cumulative nicotine release is calculated.

[0143] Table 2 shows the cumulative nicotine release over time for oral nicotine pouch products P2, A1, and A2. Product P2 exhibits slow release within 60 seconds, achieving a cumulative release rate of 81% or higher at 2100 seconds, demonstrating both slow release and a high cumulative release rate. In the comparative example, product A1 releases rapidly between 30 and 40 seconds, reaching a release rate of 24.58% at 40 seconds; product A2 releases rapidly within 10 seconds, reaching a release rate of 9.93% at 10 seconds. Both A1 and A2 show relatively low cumulative release rates at 2100 seconds, less than 80%. At higher pH levels, this rapid release disrupts the acid-base balance of the oral mucosa, leading to oral discomfort and a reduced nicotine experience.

[0144] Table 2. Statistics on cumulative nicotine release and release rate in nicotine pouch products.

[0145] Test Example 3

[0146] Nicotine release experiments were conducted on oral nicotine pouch product P3 (containing 500 mg of contents per pouch, of which nicotine content is 3 mg per pouch) prepared in Example 3, oral nicotine pouch product A3 in Comparative Example 3 and oral nicotine pouch product A4 in Comparative Example 4, which have the same contents and nicotine content.

[0147] The specific method is as follows: 100 mL of simulated artificial saliva with a pH of 6.8 is placed in each beaker and maintained at 37.0±0.1℃. A nicotine sachet with the same nicotine content is placed in each beaker, and the mixture is stirred at 100 rpm. A precise sample of 2 mL is taken every minute until 10 minutes have elapsed. After 10 minutes, a sample is taken every 10 minutes, with 2 mL of simulated artificial saliva added after each sample (to simulate the cumulative nicotine release in the oral cavity, artificial saliva needs to be added after each sample as saliva is continuously secreted). The 2 mL solution is then diluted to 10 mL with simulated artificial saliva. The nicotine content is detected using HPLC, and the relative cumulative nicotine release is calculated.

[0148] Table 3 shows the cumulative nicotine release over time for oral nicotine pouch products P3, A3, and A4. Product P3 exhibits a gradual release over 2100 seconds, with a cumulative release rate of 95% or higher at 2100 seconds, achieving a slow release with a high cumulative release rate. In the comparative example, product A3 showed a release rate of 90.77% at 2100 seconds, while product A4 showed a release rate of 88.43%. Since the pH values ​​of A3 and A4 are significantly higher than those of P3, they disrupt the acid-base balance of the oral mucosa, leading to a reduced nicotine experience during oral release.

[0149] Table 3. Statistical table of cumulative nicotine release and release rate in nicotine pouch products.

[0150] Test Example 4: Taste Test

[0151] The taste test method is as follows: a professional evaluation team (n=5) will conduct the evaluation, and P2, A1 and A2, P3, A3 and A4 will be placed directly between the upper lip and the upper teeth. The standard consumption time is set at 30 minutes.

[0152] The evaluation was conducted based on visual characteristics, olfactory characteristics, gustatory characteristics, and overall experience. The evaluation grading is shown in Table 4. Table 4 Taste Test Evaluation Grading Table

[0153] (1) Taste test scores were conducted on the oral nicotine pouch products P2, A1, and A2. The results are shown in Table 5. The overall score of the oral nicotine pouch product P2 was higher than that of A1 and A2. While retaining the appearance, color, and basic taste, the flavor intensity of the oral nicotine pouch product P2 was better than that of A1 and A2, and the irritation in the oral cavity was much less than that of A1 and A2, resulting in a higher level of taste comfort.

[0154] Table 5 Taste Test Scoring Table for Oral Nicotine Pouch Products P2, A1, and A2

[0155] (2) The taste test scores of oral nicotine pouch products P3, A3, and A4 were compared and are shown in Table 6. The overall score of oral nicotine pouch product P3 was higher than that of A3 and A4. While retaining the appearance, color, and basic taste, oral nicotine pouch product P3 had better flavor persistence and aftertaste than A3 and A4, and its irritation in the oral cavity was much less than that of A3 and A4, resulting in a higher level of taste comfort.

[0156] Table 6 Taste Test Scoring Table for Oral Nicotine Pouch Products P3, A3, and A4

[0157] Therefore, it can be concluded that this patent provides a nicotine pouch product and its preparation method, which optimizes the pH value of the nicotine pouch product to a weakly acidic range (pH<6.0), thereby achieving efficient nicotine release. This aims to solve the problems of oral irritation, limited flavor, and strong pH dependence of existing nicotine pouches during use, improve the palatability of nicotine pouches during use, increase the nicotine release efficiency during oral consumption, achieve long-term stable nicotine delivery by controlling release kinetics, reduce production costs, and enhance the consumer experience.

[0158] In the foregoing description of exemplary embodiments / specific implementations of this patent, various features of this patent are sometimes combined in a single embodiment / specific implementation or its figures and description, with the aim of simplifying the disclosure and aiding in the understanding of one or more of the various aspects of the invention. However, unless expressly stated otherwise or in obvious technical contradiction or exclusion, the descriptive method of this patent should not be construed as reflecting an intention that the claimed features of the invention are more than expressly stated in each claim. Rather, the inventive aspect reflected in the claims lies in not all the features of a single foregoing disclosed embodiment / specific implementation. Therefore, the claims following the detailed description are hereby expressly incorporated into this detailed description, each claim existing independently as a separate embodiment / specific implementation of this patent.

[0159] The terms and expressions used in this specification are for illustrative purposes and not for limitation. Their use is not intended to exclude any equivalents of the shown and described features or portions thereof, but rather to facilitate the understanding that various modifications may be possible within the scope of this patent claim. Therefore, it should be understood that while this patent has been specifically disclosed through preferred embodiments, exemplary embodiments, and optional features, variations or modifications of the concepts disclosed herein may be adopted by those skilled in the art, and such variations and modifications are therefore considered to be within the scope of this patent as defined by the appended claims.

[0160] The specific implementations given in this specification are examples of useful implementations of this patent. It will be apparent to those skilled in the art that this patent can be implemented using many variations of the equipment, equipment components, and method steps disclosed in this specification.

[0161] The foregoing description of specific embodiments fully discloses the general features of this patent, enabling others to easily modify and / or adapt such embodiments for various applications by applying knowledge within the scope of the art, without excessive experimentation or deviation from the general concept of this patent. Therefore, based on the teachings and guidance provided herein, it is intended that such modifications and alterations be included within the meaning and scope of equivalents of the disclosed embodiments. It should be understood that the wording or terminology used herein is for descriptive purposes and not intended to be limiting; thus, the wording or terminology in this specification will be interpreted by those skilled in the art based on the foregoing teachings and guidance.

[0162] Furthermore, the scope of this patent should not be limited to any of the exemplary embodiments described above, but only to the appended claims and their equivalents.

Claims

1. A nicotine-filled pouch product, characterized in that, The oral nicotine pouch product includes the contents and the outer packaging; The contents are in powder form and include a nicotine source and an acidic pH adjuster; The outer packaging is a saliva-permeable pouch used to encapsulate the contents, such that the pH value of the oral nicotine pouch product is <6.0 in pure water or saliva.

2. The oral nicotine pouch product according to claim 1, characterized in that, The amount of the acidic pH adjuster added is 2.0~3.0%, 3.0~5.0%, 5.0~7.0%, or 7.0~9.0%; the acidic pH adjuster includes one or more combinations of organic acids, organic acid salts, or inorganic acid salts; The organic acids include one or more combinations of citric acid, malic acid, lactic acid, acetic acid, tartaric acid, gluconic acid, or fumaric acid. The organic acid salts include one or more combinations of alkali metal or ammonium citrate, malate, lactate, tartrate, gluconate or fumarate; The inorganic acid salts include one or more combinations of alkali metal or ammonium carbonates, acetates, monohydrogen phosphates, dihydrogen phosphates, trihydrogen phosphates, or bicarbonates.

3. The oral nicotine pouch product according to claim 1, characterized in that, The amount of nicotine source added is 1.0~2.0%, 2.0~3.0%, or 3.0~4.0%, and the nicotine source includes one or more combinations of free nicotine salts or elemental nicotine. The free nicotine salts include one or more combinations of nicotine hydrochloride, nicotine dihydrochloride, nicotine citrate, nicotine monotartrate, nicotine hydrogen tartrate, nicotine hydrogen tartrate dihydrate, nicotine sulfate, nicotine resinate, and nicotine salicylate.

4. The oral nicotine pouch product according to claim 1, characterized in that, The contents also include a filler, the filler having a water content ≤7.0%, and the filler having a particle size of 15~30 μm, 30~50 μm, 50~80 μm, 80~120 μm or 120~200 μm.

5. The oral nicotine pouch product according to claim 4, characterized in that, The filler is a porous matrix, which is plant fiber or cellulose derivative; The cellulose derivatives include one or more combinations of hydrolyzed cellulose, cellulose ether, cellulose ester or cellulose ether ester; The hydrolyzed cellulose includes microcrystalline cellulose; The cellulose esters include one or more combinations of cellulose nitrate, cellulose acetate, cellulose acetate butyrate, or cellulose xanthate. The cellulose ethers include one or more combinations of methylcellulose, carboxymethylcellulose, ethylcellulose, hydroxyethylcellulose, cyanoethylcellulose, hydroxypropylcellulose, or hydroxypropylmethylcellulose.

6. The oral nicotine pouch product according to claim 1, characterized in that, The contents also include excipients, sweeteners, and flavorings; The amount of the excipient added is 0.1~1.0%, 1.0~2.0%, or 2.0~3.0%; the excipient includes one or more combinations of silicon dioxide, calcium silicate, calcium stearate, magnesium stearate, sodium alginate, and sodium carboxymethyl cellulose. The amount of sweetener added is 0.5~2.0%, 2.0~5.0%, or 5.0~10.0%; the particle size of the sweetener is 50~80μm, 80~120μm, 120~180μm, or 180~250μm. The amount of flavoring and fragrance added is 2.0~4.0%, 4.0~7.0%, or 7.0~10.0%.

7. The oral nicotine pouch product according to any one of claims 1 to 6, characterized in that, The filling amount of the contents in the oral nicotine pouch product is 100-300 mg, 300-500 mg, 500-800 mg, 800-1200 mg, or 1200-1500 mg; the nicotine content in the contents is 0.1-1.0 mg, 1.0-3.0 mg, 3.0-5.0 mg, 5.0-8.0 mg, or 8.0-15.0 mg.

8. A method for preparing a nicotine-containing pouch product according to claim 7, characterized in that, Includes the following steps: Step A: Mix the filler and sweetener to obtain a premix; add the nicotine source and excipient to the premix, mix evenly to obtain a solid mixture; Step B: Add an acidic pH adjuster aqueous solution and fragrance to the solid mixture, mix well, and then sieve to obtain the contents; Step C: Fill the outer packaging with the contents, seal the edges and sterilize with ultraviolet light to obtain the oral nicotine pouch product.

9. The method for preparing the oral nicotine pouch product according to claim 8, characterized in that, In step A, the mass ratio of the filler to the sweetener is (3.0~10.0):1; In step B, the aqueous solution of the acidic pH adjuster is added to the solid mixture by spraying.

10. The method for preparing the oral nicotine pouch product according to claim 9, characterized in that, The oral nicotine pouch product has a cumulative nicotine release rate of >81% in the oral cavity from 0 to 35 minutes.

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