Bagged nicotine product in mouth and preparation method thereof

Abstract

The invention discloses a buccal bagged nicotine product and a preparation method thereof, and is characterized in that the buccal bagged nicotine product comprises a content and an outer package, and the content is packaged in the outer package; the content comprises a matrix composition and at least one rupturable capsule; the rupturable capsule releases the liquid-phase content under the action of pressure, and the liquid-phase content is in contact with the nicotine source in the matrix composition to increase the pH value, so that the nicotine source in the matrix composition is rapidly released. Therefore, on the premise that the long-term storage stability of the product is not sacrificed, the problems that an existing buccal bagged nicotine product is rough in mouth feel in the oral cavity, nicotine is slow in head rising and the sensory experience of a user is poor are solved, the nicotine release rate and the sensory experience of the buccal bagged nicotine product during buccal consumption are improved, and the production cost is reduced.

Description

Technical Field

[0001] This patent belongs to the field of oral tobacco products technology, specifically relating to an oral nicotine bagged product and its preparation method. Background Technology

[0002] With the continuous advancement of global tobacco control policies and the increasing health awareness of consumers, countries are adopting different strategies to achieve smoke-free goals. Smokeless tobacco products, as the only tobacco products that can be used in any public place, are a powerful alternative to traditional cigarettes. Smokeless nicotine products are mainly divided into snuff, nicotine-containing products, chewing tobacco, and other products. Sales are gradually increasing in many countries. Among them, nicotine-containing products have a much lower N-nitrosamine (TSNA) content than traditional cigarettes, making them far less harmful. Nicotine-containing products are mostly available in pouches, while the domestic market for smokeless nicotine products is still in its early stages.

[0003] Oral nicotine products, such as nicotine pouches, are a new type of smokeless tobacco product that allows nicotine to be absorbed through the oral mucosa. Their typical structure usually includes a pouch made of a saliva-permeable packaging material, and a filler material sealed inside the pouch. This filler material generally contains components such as a nicotine source (e.g., nicotine salts), fillers, pH adjusters, and flavoring agents. In existing technologies, pH adjusters (e.g., sodium carbonate, sodium bicarbonate, sodium hydroxide, etc.) are usually physically mixed with the nicotine source and other components in the form of a solid powder. After saliva permeates into the pouch, it dissolves the pH adjuster powder, raising the pH value of the local microenvironment, causing the protonated nicotine salts to convert into free nicotine. Because free nicotine has higher lipid solubility, it is more easily absorbed by the body through the oral mucosa.

[0004] For example, patent document CN119699630A discloses a sustained-release nicotine lozenge and its preparation method, which achieves a sustained-release effect by encapsulating nicotine / salt and flavoring in a sustained-release adjuvant; patent document CN116268530A discloses a nicotine lozenge containing a pH-adjusting inclusion complex and its preparation method, which forms a pH-adjusting inclusion complex by mixing γ-cyclodextrin with a pH-adjusting solution and freeze-drying it to allow the pH-adjusting agent to be released slowly and is not easily oxidized during storage; patent document CN119745100A discloses a temperature-sensitive controlled-release lozenge and its preparation method, which obtains a mixed system by adding a saturated sodium carbonate aqueous solution to an ethanol phase containing cocoa butter, drying and pulverizing it to prepare a temperature-sensitive pH-adjusting microcapsule, which is then rapidly released in the oral cavity to achieve a pH of 8-9. However, the pH adjusters in the three patent applications mentioned above are all solid. Their dissolution and ion diffusion processes will result in a significant lag effect in the conversion and release of nicotine, making it difficult to achieve rapid onset of action. Users need to wait at least 3-5 minutes to perceive the effect. Furthermore, the pH adjuster is prone to adverse chemical reactions with nicotine and other flavor substances during storage, leading to raw material degradation or quality changes, thus affecting the shelf-life stability of nicotine oral products. Additionally, it has a rough taste in the mouth, resulting in a poor user experience.

[0005] Therefore, there is an urgent need to develop a nicotine product in a sachet that can solve the problems of rough taste in the mouth, slow nicotine onset, and poor sensory experience of existing nicotine products in a sachet without sacrificing the long-term storage stability of the product. This would improve the nicotine release rate and sensory experience when consuming nicotine products in a sachet, and reduce production costs. Summary of the Invention

[0006] The purpose of this patent is to provide a nicotine product in a sachet and its preparation method, which solves the problems of rough taste in the mouth, slow nicotine onset, and poor sensory experience of existing nicotine products in a sachet without sacrificing the long-term storage stability of the product. The goal is to achieve rapid nicotine release, strong sensory experience, and low production cost when the nicotine product is consumed in the mouth.

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

[0008] A nicotine product in a sachet includes contents and an outer packaging, wherein the contents are encapsulated within the outer packaging; the contents include a matrix composition and at least one ruptureable capsule; the ruptureable capsule releases liquid contents under pressure, and the liquid contents contact the nicotine source in the matrix composition to increase the pH value, thereby rapidly releasing the nicotine source in the matrix composition.

[0009] Furthermore, the liquid phase contents are an aqueous solution of a pH adjuster, which is an alkaline aqueous solution.

[0010] Furthermore, the pH adjusting aqueous solution includes one or more combinations of sodium orthophosphate, potassium orthophosphate, calcium orthophosphate, sodium diphosphate, potassium diphosphate, calcium diphosphate, pentasodium triphosphate, pentapotassium triphosphate, sodium polyphosphate, potassium polyphosphate, carbonic acid, sodium carbonate, sodium bicarbonate, potassium carbonate, calcium carbonate, magnesium carbonate, magnesium oxide, or metal hydroxide.

[0011] Furthermore, the concentration of the pH adjuster aqueous solution is 5-8%, 8-12%, 12-15%, 15-20%, or 20-25%.

[0012] Furthermore, the diameter of the ruptureable capsule is 1.5~1.8 mm, 1.8~2.2 mm, or 2.2~2.5 mm;

[0013] Furthermore, the water content of the ruptureable capsules is 10-12%, 12-14%, or 14-15%.

[0014] Furthermore, the ruptureable capsule also includes a shell, which is a soft capsule body used to encapsulate the liquid contents.

[0015] Furthermore, the outer shell includes a gelling agent and a humectant, with the gelling agent and humectant added in a mass ratio of 1:(1~3).

[0016] Furthermore, the gelling agent includes one or more combinations of gelatin, agar, konjac polysaccharide, xanthan gum, pectin, carrageenan, sodium alginate, psyllium husk, guar gum, gellan gum, guar gum, whey protein, casein, or soy protein.

[0017] Furthermore, the humectants include one or more combinations of glycerin, propylene glycol, xylitol, sorbitol, maltodextrin, NCS, D-galacturonic acid pyranoside, chitosan derivatives, and PDSI-101.

[0018] Furthermore, the matrix composition is in powder form, and the nicotine content of the nicotine source in the matrix composition is 2-3% (w / w), 3-5% (w / w), or 5-6% (w / w).

[0019] Furthermore, nicotine sources include one or more combinations of free nicotine, nicotine salts, nicotine-ion exchange resins, nicotine complexes, and non-covalently bound nicotine.

[0020] Furthermore, free nicotine includes tobacco extracts; nicotine salts include one or more combinations of nicotine malate, nicotine citrate, nicotine tartrate, nicotine salicylate, nicotine benzoate, nicotine sulfate, and nicotine cyclodextrin-encapsulated complexes; nicotine-ion exchange resins include acidic ion exchange resins, which include strongly acidic cation exchange resins or weakly acidic cation exchange resins, with strongly acidic cation exchange resins including one or more combinations of styrene-based strongly acidic ion exchange resins and macroporous strongly acidic ion exchange resins; and weakly acidic cation exchange resins include one or more combinations of isobutyrate ion exchange resins, acrylic acid ion exchange resins, and 724 weakly acidic ion exchange resins.

[0021] Furthermore, the matrix composition also includes a release control agent and a cellulose derivative.

[0022] Furthermore, the release control agents include one or a combination of two of magnesium stearate, calcium stearate, and silicon dioxide.

[0023] Furthermore, cellulose derivatives include one or more combinations of cellulose ethers, cellulose esters, or cellulose ether esters.

[0024] Furthermore, cellulose esters include cellulose nitrates, cellulose acetates, cellulose acetate butyrate, or cellulose xanthate; cellulose ethers include methylcellulose, carboxymethylcellulose, ethylcellulose, hydroxyethylcellulose, cyanoethylcellulose, hydroxypropylcellulose, or hydroxypropylmethylcellulose.

[0025] Alternatively, the matrix composition may also include flavorings and fragrances.

[0026] Furthermore, the flavorings and fragrances are non-exhaustive examples, 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, 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 contain essential oils, including peppermint, spearmint, menthol, eucalyptus, clove oil, laurel oil, fennel, thyme, cedarwood oil, nutmeg, and oils from the aforementioned fruits.

[0027] This patent also provides a method for preparing a nicotine product in a sachet, comprising the following steps:

[0028] Step A: Dissolve the pH adjuster in pure water to obtain liquid contents, and encapsulate the liquid contents in an outer shell to obtain a ruptureable capsule;

[0029] Step B: Mix the nicotine source and the filler evenly to obtain a matrix composition; disperse at least one ruptureable capsule in the matrix composition to obtain the contents;

[0030] Step C: The contents are sealed in an outer packaging and sterilized with ultraviolet light to form a nicotine product in a lozenge.

[0031] Furthermore, in step B, the filler includes a release control agent, a cellulose derivative, a sweetener, and a flavoring; the mass ratio of the ruptureable capsule to the matrix composition in the contents is (1.0~2.0):(8.0~9.0);

[0032] Furthermore, in step C, the outer packaging is a saliva-permeable pouch, which may be made of medical-grade nonwoven fabric, Lyocell, Modal, or Tencel, and the quantitative amount of the saliva-permeable pouch is 25~35 g / m³. 2 .

[0033] Furthermore, the release rate of nicotine from a nicotine pouch in the oral cavity is ≥40% within 0 to 120 seconds.

[0034] Furthermore, nicotine products in oral pouches can be stored at room temperature for at least 180 days.

[0035] The outer packaging may also include flavorings and fragrances for added aroma.

[0036] As used in this patent, "oral nicotine products in pouches" generally refers to oral smokeless tobacco products that are placed between the lips and gums and release some of the soluble substances through saliva.

[0037] As used in this patent, "nicotine" (also known as nicotine alkaloid) has the chemical formula C. 10 H 14 N2 is a pyridine alkaloid. In this text, the terms "nicotine" and "nicotine alkaloid" are used interchangeably.

[0038] Compared with existing technologies, the oral nicotine pouch product and its preparation method provided by this patent have the following beneficial technical effects:

[0039] (1) By pre-dissolving an alkaline pH adjuster in the liquid contents of the capsule, when the user chews or takes the oral nicotine composition in a sachet, the capsule ruptures under physical pressure, releasing a high concentration of alkaline aqueous solution. This alkaline aqueous solution then immediately comes into contact with the nicotine source in the matrix composition, acting instantly on the nicotine source particles, shortening the alkalization time of the raw materials and accelerating the initial release rate. In vitro nicotine release experiments verified that the nicotine release of the product of this invention accounts for 45%-50% of the total content within 1 minute, while existing solid pH adjuster products release 15%-0%; volunteer taste tests showed that the average onset time of the product of this invention is 45-60 seconds, which is significantly shorter than that of existing products (3-5 minutes).

[0040] (2) Improve product stability: During the storage period, the highly active alkaline solution is isolated in a sealed capsule, avoiding direct contact with other components, thereby reducing the risk of stability problems such as raw material degradation, volatilization or clumping.

[0041] (3) Provide sensory feedback: When the capsule breaks under oral pressure, the trace amount of water released can moisten the dry powder matrix. The physical breaking sensation brought by chewing the capsule is also a user experience signal.

[0042] (4) Industrial feasibility: Capsules that are difficult to break can be produced using mature processes, and their filling process is compatible with existing nicotine bag production lines. Attached Figure Description

[0043] 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.

[0044] Figure 1 This is a schematic diagram of the structure of the oral nicotine bag product of this patent.

[0045] Figure 2 This is a schematic diagram of the structure of the ruptureable capsule in the oral nicotine bag product of this patent;

[0046] Figure 3 This is an in vitro nicotine release curve of the orally packaged nicotine product in the test example of this patent (where the horizontal axis is time in seconds; the vertical axis is cumulative release in %).

[0047] The reference numerals in the attached figures are as follows:

[0048] Oral nicotine products in packets: 100;

[0049] Permeable pouches: 110;

[0050] Matrix composition: 120;

[0051] Fragile capsule: 130;

[0052] Casing: 131;

[0053] Liquid phase contents: 132. Detailed Implementation

[0054] The detailed features and advantages of this application are described below in the specific embodiments. The content of this description 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, a person skilled in the art can easily understand the related objectives and advantages of this application.

[0055] In this specification and claims, several terms will be used, and unless otherwise indicated, these terms will be defined to have the following meanings:

[0056] As used in this patent, the term "pH adjuster" refers to one or more substances added for the purpose of adjusting and controlling the pH of an aqueous liquid when a product containing a pH adjuster is dissolved or dispersed in an aqueous liquid (such as saliva).

[0057] 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.

[0058] 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.

[0059] 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.

[0060] 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.

[0061] Unless otherwise specified, all embodiments and preferred embodiments mentioned herein can be combined to form new technical solutions.

[0062] Unless otherwise specified, all the technical features and preferred features mentioned herein can be combined to form new technical solutions.

[0063] 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.

[0064] 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.

[0065] 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.

[0066] 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).

[0067] Unless otherwise specified, percentages (%) in this document refer to percentages by mass relative to the composition.

[0068] Unless otherwise stated herein, the sum of the contents of the components in the composition is 100%.

[0069] 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.

[0070] Unless otherwise specified, the term "a" as used in this specification means "at least one".

[0071] 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.

[0072] 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.

[0073] 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.

[0074] This patent provides a nicotine product in a sachet and its preparation method, including the following steps:

[0075] S1. Preparation of ruptureable capsules, the specific steps are as follows:

[0076] 1. Dissolve the pH adjuster in pure water to prepare a mixed solution with a concentration of 5~25% (W / W). Filter the solution through a 0.45 μm filter membrane for later use. This is the pH adjuster aqueous solution.

[0077] The pH adjuster is an alkaline adjuster, which includes one or more combinations of sodium orthophosphate, potassium orthophosphate, calcium orthophosphate, sodium diphosphate, potassium diphosphate, calcium diphosphate, pentasodium triphosphate, pentapotassium triphosphate, sodium polyphosphate, potassium polyphosphate, carbonic acid, sodium carbonate, sodium bicarbonate, potassium carbonate, calcium carbonate, magnesium carbonate, magnesium oxide, or metal hydroxides. When there are two pH adjusters in combination, they can be dissolved in pure water at a mass ratio of 1:(1~3) to prepare a 25% (w / w) mixed solution. After filtration through a 0.45 μm filter membrane, the solution is ready for use as a pH adjuster aqueous solution.

[0078] 2. Mix the gelling agent and the moisturizing agent thoroughly at a mass ratio of 1:(1~3) to obtain the adhesive solution.

[0079] The gelling agent includes one or more combinations of gelatin, agar, konjac polysaccharide, xanthan gum, pectin, carrageenan, sodium alginate, psyllium husk, guar gum, gellan gum, gluconol, whey protein, casein, or soy protein. The humectant includes one or more combinations of glycerin, propylene glycol, xylitol, sorbitol, maltodextrin, NCS, D-galactopyranocyanate, chitosan derivatives, and PDSI-101.

[0080] 3. Place the pH-adjusting aqueous solution prepared in step 1 and the gel solution prepared in step 2 into a conventional rotary soft capsule machine and compress them into spherical or near-spherical soft capsules with a diameter of approximately 1.5~2.5 mm. The gel solution serves as the outer shell, and the pH-adjusting aqueous solution serves as the liquid content. The near-spherical soft capsules include elliptical or olive-shaped capsules.

[0081] 4. Place the spherical soft capsules prepared in step 3 above in a fluidized bed and dry them at a temperature of 27~32℃ for 2~4 h, so that the moisture content of the dried spherical soft capsules is 10~15%. Monitor the moisture content with an online moisture meter until it reaches the standard, and then obtain the ruptureable capsules.

[0082] S2. Preparation of the matrix composition, the specific steps are as follows:

[0083] According to the mass percentage, 40-60% of sweetener, 20-30% of cellulose derivative, 0.5-5.0% of nicotine source (here, 2-6% specifically refers to the nicotine content contained in the nicotine source), 0.8-1.5% of release control agent, and 0.5-1.5% of flavoring are placed in a V-type mixer and mixed for 20-40 minutes at a speed of 10-25 rpm to ensure that the above materials are free of lumps. After uniform mixing, the matrix composition is obtained.

[0084] The sweeteners include one or more combinations of aspartame, acesulfame potassium, cyclamate, saccharin, sodium saccharin, sucralose, neotame, sodium cyclohexylsulfamate, stevia, licorice, disodium glycyrrhizate, tripotassium and trisodium glycyrrhizate, glucose, fructose, sucrose, maltose, corn syrup, starch sugar and lactose, sorbitol, maltitol, isomaltitol, palaginitol, xylitol, lactitol, mannitol, erythritol or dextran.

[0085] Cellulose derivatives include one or more combinations of cellulose ethers, cellulose esters, or cellulose ether esters; cellulose esters include cellulose nitrates, cellulose acetates, cellulose acetate butyrate, or cellulose xanthates; cellulose ethers include methylcellulose, carboxymethylcellulose, ethylcellulose, hydroxyethylcellulose, cyanoethylcellulose, hydroxypropylcellulose, or hydroxypropylmethylcellulose.

[0086] Nicotine sources include one or more combinations of free nicotine, nicotine salts, nicotine-ion exchange resins, nicotine complexes, and non-covalently bound nicotine. Free nicotine includes tobacco extracts; nicotine salts include one or more combinations of nicotine malate, nicotine citrate, nicotine tartrate, nicotine salicylate, nicotine benzoate, nicotine sulfate, and nicotine cyclodextrin-encapsulated complexes; nicotine-ion exchange resins include acidic ion exchange resins, which include strongly acidic cation exchange resins or weakly acidic cation exchange resins; strongly acidic cation exchange resins include one or more combinations of styrene-based strongly acidic ion exchange resins and macroporous strongly acidic ion exchange resins; weakly acidic cation exchange resins include one or more combinations of isobutyrate ion exchange resins, acrylic acid ion exchange resins, and 724 weakly acidic ion exchange resins.

[0087] Release control agents include one or a combination of two of magnesium stearate, calcium stearate, and silica, which utilize their high specific surface area to adsorb moisture, thereby reducing the risk of clumping in the matrix composition.

[0088] 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, peppermint, deer antler, spearmint, eucalyptus, mint, and fruit flavorings (e.g., from apple, pear, peach, strawberry, apricot, raspberry, cherry, pineapple, lemongrass, lime, chili (capsaicin), citrus, tobacco flavors, bergamot, and plum). Preferably, the flavorings and fragrances also contain essential oils, including peppermint, spearmint, menthol, eucalyptus, clove oil, laurel oil, fennel, thyme, cedarwood oil, nutmeg, and oils from the aforementioned fruits.

[0089] S3. Preparation of oral nicotine pouches, the specific steps are as follows:

[0090] 1. Mix the ruptureable capsules prepared in step S1 with the matrix composition prepared in step S2 at a mass ratio of (1.0~2.0):(8.0~9.0), and gently mix them in a drum mixer for 3~8 minutes at a mixing speed of 7~11 rpm. During the mixing process, take samples every 1 minute to observe the breakage of the ruptureable capsules. The breakage rate should be controlled below 0.5% to ensure that the capsules are evenly dispersed and undamaged, thus obtaining the contents of the oral nicotine bagged product.

[0091] 2. Using an automatic filling and packaging machine, fill the outer packaging with 0.3~0.6 g of the contents of the oral nicotine product prepared in step S31 above, heat-seal it and sterilize it with ultraviolet light to obtain the oral nicotine product.

[0092] The outer packaging consists of saliva-permeable pouches, which can be made of medical-grade nonwoven fabric, lyocell, modal, or tencel. The quantitative amount of the saliva-permeable pouches can be 25~35 g / m³. 2 Among them, medical-grade nonwoven fabric is one or more combinations of polypropylene fiber, polyester fiber, polyamide fiber, polytetrafluoroethylene fiber and glass fiber.

[0093] like Figures 1-2 As shown, the oral nicotine pouch product 100 includes a saliva-permeable pouch 110 and a filling carrier completely encapsulated inside the saliva-permeable pouch 110, the filling carrier including a matrix composition 120 and a ruptureable capsule 130.

[0094] Specifically, the matrix composition 120 is a non-binding powder, and the number of ruptureable capsules 130 is one or more, uniformly dispersed in the matrix composition 120.

[0095] More specifically, the ruptureable capsule 130 includes a sealed outer shell 131 made of edible material and liquid contents 132 completely encapsulated inside the outer shell 131. When a user places the oral nicotine product 100 in their mouth and applies a chewing pressure of 8-15 N, the outer shell 131 of the ruptureable capsule 130 ruptures, and the liquid contents 132 inside the outer shell 131 are released instantaneously. This liquid contents rapidly mix with the surrounding matrix composition 120 and increase the local pH, thereby causing the nicotine source in the oral nicotine product 100 to be instantly converted into a free alkali form and rapidly absorbed.

[0096] Example 1

[0097] (1) Dissolve sodium carbonate and sodium bicarbonate in purified water at a mass ratio of 1:2 to prepare a 25% (w / w) aqueous solution. Filter the solution through a 0.45 μm filter membrane for later use to obtain the pH adjuster aqueous solution.

[0098] (2) Mix gelatin and glycerin thoroughly in a mass ratio of 1:2 to obtain a gel solution;

[0099] (3) Place the pH adjuster aqueous solution in step (1) and the gel solution in step (2) into a conventional rotary soft capsule machine and press them into spherical soft capsules with a diameter of 2.5 mm.

[0100] (4) Place the spherical soft capsules obtained in step (3) above in a fluidized bed and dry them at 30°C for 3 h so that the water content of the dried spherical soft capsules is 10±2%. The water content is monitored by an online moisture meter until it reaches the standard, and then the ruptureable capsules are obtained.

[0101] (5) According to the mass percentage, 50% sorbitol, 30% microcrystalline cellulose, 4% nicotine-polyacrylic acid resin complex (4% here specifically refers to the nicotine content), 1.0% magnesium stearate and 1.0% peppermint flavor are placed in a V-type mixer and mixed for 30 min at a speed of 15 rpm to ensure that the above materials are free of lumps. After uniform mixing, the matrix composition is obtained.

[0102] (6) The ruptureable capsules obtained in step (4) above are mixed with the matrix composition prepared in step (5) above at a ratio of 1.5:8.5, and gently mixed in a drum mixer for 5 min at a mixing speed of 8 rpm. During the mixing process, samples are taken every 1 min to observe the breakage of the ruptureable capsules. The breakage rate is controlled below 0.5% to ensure that the capsules are evenly dispersed and undamaged, and the contents of the oral nicotine bag product are obtained.

[0103] (7) Using an automatic filling and packaging machine, 0.4 g of the contents of the oral nicotine product prepared in step (6) above is filled into a saliva-permeable pouch, heat-sealed and sterilized with ultraviolet light to obtain the oral nicotine product, which is marked as P1.

[0104] Example 2

[0105] (1) Dissolve sodium carbonate and potassium carbonate in purified water at a mass ratio of 1:2 to prepare a 25% (w / w) aqueous solution. Filter the solution through a 0.45 μm filter membrane for later use to obtain the pH adjuster aqueous solution.

[0106] (2) Mix pectin and propylene glycol thoroughly at a mass ratio of 1:3 to obtain a gel solution;

[0107] (3) Place the pH adjuster aqueous solution in step (1) and the gel solution in step (2) into a conventional rotary soft capsule machine and press them into spherical soft capsules with a diameter of 2.5 mm.

[0108] (4) Place the spherical soft capsules obtained in step (3) above in a fluidized bed and dry them at 30°C for 3 h so that the water content of the dried spherical soft capsules is 10±2%. The water content is monitored by an online moisture meter until it reaches the standard, and then the ruptureable capsules are obtained.

[0109] (5) According to the mass percentage, 45% maltitol, 35% microcrystalline cellulose, 5% nicotine-polyacrylic acid resin complex (5% here specifically refers to the nicotine content), 0.8% magnesium stearate and 1.0% lemon flavor are placed in a V-type mixer and mixed for 30 min at a speed of 15 rpm to ensure that the above materials are free of lumps. After uniform mixing, the matrix composition is obtained.

[0110] (6) The ruptureable capsules obtained in step (4) above are mixed with the matrix composition prepared in step (5) above at a ratio of 1.5:8.5, and gently mixed in a drum mixer for 5 min at a mixing speed of 8 rpm. During the mixing process, samples are taken every 1 min to observe the breakage of the ruptureable capsules. The breakage rate is controlled below 0.5% to ensure that the capsules are evenly dispersed and undamaged, and the contents of the oral nicotine bag product are obtained.

[0111] (7) Using an automatic filling and packaging machine, 0.4 g of the contents of the oral nicotine product prepared in step (6) above is filled into a saliva-permeable pouch, heat-sealed and sterilized with ultraviolet light to obtain the oral nicotine product, which is marked as P2.

[0112] Example 3

[0113] (1) Dissolve potassium carbonate and potassium polyphosphate in purified water at a mass ratio of 1:2 to prepare a 25% (w / w) aqueous solution. Filter the solution through a 0.45 μm filter membrane for later use to obtain the pH adjuster aqueous solution.

[0114] (2) Mix carrageenan and propylene glycol thoroughly at a mass ratio of 1:2 to obtain a glue solution;

[0115] (3) Place the pH adjuster aqueous solution in step (1) and the gel solution in step (2) into a conventional rotary soft capsule machine and press them into spherical soft capsules with a diameter of 2.5 mm.

[0116] (4) Place the spherical soft capsules obtained in step (3) above in a fluidized bed and dry them at 30°C for 3 h so that the water content of the dried spherical soft capsules is 10±2%. The water content is monitored by an online moisture meter until it reaches the standard, and then the ruptureable capsules are obtained.

[0117] (5) According to the mass percentage, 50% mannitol, 30% microcrystalline cellulose, 4% nicotine-polyacrylic acid resin complex (4% here specifically refers to the nicotine content), 1.0% silica and 1.2% cherry flavor are placed in a V-type mixer and mixed for 25 min at a speed of 15 rpm to ensure that the above materials are free of lumps. After uniform mixing, the matrix composition is obtained.

[0118] (6) The ruptureable capsules obtained in step (4) above are mixed with the matrix composition prepared in step (5) above at a ratio of 1.5:8.5, and gently mixed in a drum mixer for 5 min at a mixing speed of 8 rpm. During the mixing process, samples are taken every 1 min to observe the breakage of the ruptureable capsules. The breakage rate is controlled below 0.5% to ensure that the capsules are evenly dispersed and undamaged, and the contents of the oral nicotine bag product are obtained.

[0119] (7) Using an automatic filling and packaging machine, 0.4 g of the contents of the oral nicotine product prepared in step (6) above is filled into a saliva-permeable pouch, heat-sealed and sterilized with ultraviolet light to obtain the oral nicotine product, which is marked as P3.

[0120] Comparative Example 1

[0121] The difference between this comparative example and Example 1 is that it does not contain ruptureable capsules, but instead adds an equal amount of pH adjuster to the matrix composition. The remaining matrix composition components and weights are the same as in Example 1. The oral nicotine bag product is prepared and labeled as A1.

[0122] Comparative Example 2

[0123] The difference between this comparative example and Example 2 is that it does not contain ruptureable capsules, but instead adds an equal amount of pH adjuster to the matrix composition. The remaining matrix composition components and weights are the same as in Example 2. The oral nicotine bag product is prepared and labeled as A2.

[0124] Comparative Example 3

[0125] Compared with Example 3, the difference in this comparative example is that the matrix composition does not contain ruptureable capsules, but an equal amount of pH adjuster is added to the matrix composition. The remaining matrix composition components and weights are the same as in Example 3, and a nicotine product in a pouch is prepared and labeled as A3.

[0126] Comparative Example 4

[0127] The difference between this comparative example and Example 1 is that the ruptureable capsule and the matrix composition were mixed in a ratio of 3:7 to prepare a nicotine product in a sachet, labeled A4.

[0128] Comparative Example 5

[0129] The difference between this comparative example and Example 1 is that the ruptureable capsule and the matrix composition were mixed in a ratio of 0.5:9.5 to prepare an oral nicotine bag product, labeled A5.

[0130] Test Example 1: Nicotine In Vitro Release Test

[0131] To further illustrate the advantages of this patent, in vitro nicotine release tests were conducted on the oral nicotine products in Examples 1-3 and Comparative Examples 1-5.

[0132] (1) Artificial saliva was prepared according to conventional experimental methods: Sodium carboxymethyl cellulose was added to 700 mL of distilled water and soaked overnight. After swelling, sorbitol, sodium chloride, magnesium chloride, potassium chloride, and parabens were added (the above reagents). After dissolving, calcium phosphate and sodium phosphate solutions were added, and distilled water was added to the required volume. After stirring, the pH was adjusted to 7 with 0.01% hydrochloric acid or 0.05% sodium hydroxide. Finally, the relevant enzymes were added, and their concentrations were adjusted to α-amylase: 50–500 U / mL; lysozyme: 1–10 μg / mL; lipase: 0.5 U / mL; peroxidase: 0.5 U / mL. The saliva was bottled and sterilized with flowing steam at 100 degrees Celsius for 30 minutes. The saliva prepared in this way was a colorless, semi-transparent liquid with a salty taste and a certain viscosity.

[0133] Among them, sorbitol, potassium chloride, sodium chloride, magnesium chloride, calcium phosphate, sodium phosphate, parabens, hydrochloric acid, sodium hydroxide, α-amylase, lysozyme, lipase and peroxidase were purchased from Wuhan Sewell Biotechnology Co., Ltd., China.

[0134] (2) Take the oral nicotine products from Examples 1-3 and Comparative Examples 1-5 above and place them in 200 mL of artificial saliva with a pH of 6.8-7.0. Maintain a constant temperature of 37.0±0.1℃ and stir at a speed of 100 rpm. Take 2 mL of sample precisely every 1 minute for a total of 10 minutes. After sampling, add 2 mL of simulated artificial saliva (to simulate the cumulative release of nicotine in the oral environment, artificial saliva needs to be added after sampling as saliva is continuously secreted in the oral cavity). Dilute the 2 mL solution to 10 mL with simulated artificial saliva. Detect the nicotine content using HPLC (high performance liquid chromatography) and calculate the relative cumulative release of nicotine. Plot the release curve with the relative cumulative release as the ordinate and time as the abscissa (tested according to the current standard of artificial saliva GB / T18886-2019).

[0135] The results are as follows Figure 3 As shown, the cumulative nicotine leaching content of the oral nicotine pouch products prepared by the methods described in Examples 1-3 of this application is significantly greater than that of Comparative Examples 1-5. Specifically, the nicotine release rate of Examples 1-3 is significantly better than that of Comparative Examples 1-3, exhibiting rapid initial release, meeting the key requirement of rapid release from a proprietary nicotine source, and the overall release curve is stable, adapting to users' oral habits. Comparative Examples 1-3, which utilize existing solid pH adjuster technology, show a significant release lag, failing to address the slow onset of symptoms in traditional products. Comparative Example 4 exhibits rapid initial release, while Comparative Example 5 shows insufficient release, failing to achieve optimal results.

[0136] Test Example 2: Sensory Test

[0137] Sensory tests were conducted on the oral nicotine products in Examples 1-3 and Comparative Examples 1-5. The taste tests were divided into real-time sensory tests and sensory tests after 180 days of storage.

[0138] The taste test method is as follows: a professional evaluation team (n=5) will conduct the evaluation and place the above-mentioned oral nicotine product directly between the upper lip and the upper teeth. The standard consumption time is set at 10 minutes.

[0139] The scoring criteria are as follows:

[0140] Using a 10-point scale, roughness is rated from 1 to extremely rough, and from 10 to extremely smooth. Nicotine irritation and flavor persistence are rated from 1 to very weak / none, and from 10 to extremely strong.

[0141] The results are shown in Table 1. In terms of the change in roughness, Examples 1-3 had high roughness scores at 0 days and 180 days of storage, and the change was small, indicating that they had a delicate taste and good taste stability after long-term storage. In contrast, Comparative Examples 1-3 showed a significant decrease in roughness scores after storage, and the taste deteriorated.

[0142] In terms of flavor persistence retention, Examples 1-3 showed a small decrease in flavor persistence score after 180 days of storage, indicating a high retention rate and the ability to maintain a good flavor over a long period. In contrast, Comparative Examples 1-3 showed a low retention rate and were prone to flavor loss.

[0143] In terms of the stability of nicotine irritation, the nicotine irritation scores of Examples 1-3 did not change much before and after storage, indicating good stability; the irritation of Comparative Examples 1-3 and 5 decreased significantly after storage, and although Comparative Example 4 had a higher irritation, its alkalinity affected the taste.

[0144] Table 1. Sensory rating table for oral nicotine products in different embodiments and comparative examples.

[0145] Therefore, it can be concluded that the oral nicotine bag product and its preparation method provided by this patent have the following beneficial technical effects:

[0146] (1) By pre-dissolving an alkaline pH adjuster in the liquid contents of the capsule, when the user chews or takes the oral nicotine composition in a sachet, the capsule ruptures under physical pressure, releasing a high-concentration alkaline aqueous solution. This alkaline aqueous solution then immediately comes into contact with the nicotine source in the matrix composition, acting instantly on the nicotine source particles, shortening the alkalization time of the raw materials and accelerating the initial release rate. In vitro nicotine release experiments verified that the nicotine release of the product of this invention accounts for 40%~50% of the total content within 2 minutes, while existing solid pH adjuster products release 15~20%; volunteer taste tests showed that the average onset time of the product of this invention is 45~120 seconds, which is significantly shorter than that of existing products (3~5 minutes).

[0147] (2) Improve product stability: During the storage period, the highly active alkaline solution is isolated in a sealed capsule, avoiding direct contact with other components, thereby reducing the risk of stability problems such as raw material degradation, volatilization or clumping.

[0148] (3) Provide sensory feedback: When the capsule breaks under oral pressure, the trace amount of water released can moisten the dry powder matrix. The physical breaking sensation brought by chewing the capsule is also a user experience signal.

[0149] (4) Industrial feasibility: Capsules that are difficult to break can be produced using mature processes, and their filling process is compatible with existing nicotine bag production lines.

[0150] 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.

[0151] 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. The specific embodiments given in this specification are examples of useful embodiments of this patent, and it will be apparent to those skilled in the art that this patent can be implemented using many variations of the devices, device components, and method steps disclosed herein.

[0152] 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.

[0153] 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 bag-in-mouth nicotine product, characterized in that, The bag-in-mouth nicotine product comprises a content and an outer package, the content is packaged in the outer package; The content comprises a matrix composition and at least one breakable capsule; the breakable capsule releases a liquid phase content under the action of pressure, and the liquid phase content contacts the nicotine source in the matrix composition to increase the pH value, so that the nicotine source in the matrix composition is rapidly released.

2. The pouched nicotine product of claim 1, wherein, The liquid phase content is an aqueous solution of a pH regulator, the aqueous solution of the pH regulator is an alkaline aqueous solution, The aqueous solution of the pH regulator comprises one or more combinations of sodium orthophosphate, potassium orthophosphate, calcium orthophosphate, sodium diphosphate, potassium diphosphate, calcium diphosphate, pentasodium triphosphate, pentapotassium triphosphate, sodium polyphosphate, potassium polyphosphate, carbonic acid, sodium carbonate, sodium bicarbonate, potassium carbonate, calcium carbonate, magnesium carbonate, magnesium oxide or metal hydroxide.

3. The mouth pouch nicotine product of claim 2, wherein, The concentration of the aqueous solution of the pH regulator is 5-8%, 8-12%, 12-15%, 15-20% or 20-25%.

4. The bag-in-mouth nicotine product according to claim 3, wherein The diameter of the breakable capsule is 1.5-1.8 mm, 1.8-2.2 mm or 2.2-2.5 mm; The water content of the breakable capsule is 10-12%, 12-14% or 14-15%; The breakable capsule further comprises a shell, and the shell is a soft capsule body for packaging the liquid phase content.

5. The bag-in-mouth nicotine product according to claim 4, wherein The shell comprises a gelling agent and a humectant, and the gelling agent and the humectant are added in a mass ratio of 1:(1-3); The gelling agent comprises one or more combinations of gelatin, agar, konjac polysaccharide, xanthan gum, pectin, carrageenan, sodium alginate, psyllium polysaccharide, guar gum, gellan gum, pullulan, whey protein, casein or soybean protein; The humectant comprises one or more combinations of glycerol, propylene glycol, xylitol, sorbitol, maltoligosaccharide alcohol, NCS, D-galacturonic acid, chitosan derivative and PDSI-101.

6. The pouched nicotine product of claim 1, wherein, The matrix composition is in powder form, and the content of nicotine in the nicotine source in the matrix composition is 2-3% (w / w), 3-5% (w / w) or 5-6% (w / w); The nicotine source comprises one or more combinations of free nicotine, nicotine salt, nicotine-ion exchange resin, nicotine complex and non-covalently bound nicotine.

7. The plug-in pouch nicotine product of claim 6, wherein, The matrix composition further comprises a release control agent and a cellulose derivative; The release control agent comprises one or a combination of magnesium stearate, calcium stearate and silicon dioxide; The cellulose derivative comprises one or more combinations of cellulose ether, cellulose ester or cellulose ether ester.

8. A method of making a pouchable nicotine product according to any one of claims 1 to 7, wherein, The method comprises the following steps: Step A: dissolving a pH regulator into pure water to obtain the liquid phase content, and packaging the liquid phase content in a shell to obtain the breakable capsule; Step B: uniformly mixing the nicotine source and a filler to obtain the matrix composition; dispersing at least one of the breakable capsules in the base composition to obtain the content; Step C: packaging the content in the outer package to form the pouchable nicotine product after ultraviolet sterilization.

9. The method for preparing the pouchable nicotine product according to claim 8, characterized in that, in step B, the filler includes a release control agent, a cellulose derivative, a sweetener, and a flavoring agent; and the mass ratio of the breakable capsules to the base composition in the content is (1.0-2.0):(8.0-9.0); In step C, the overwrap is a saliva permeable pouch comprising a medical grade nonwoven, lyocell, modal or tencel, the saliva permeable pouch having a basis weight of 25-35 g / m 2 .

10. A method of making a mouth pouch nicotine product according to claim 9, characterised in that, the release amount of the pouchable nicotine product in the oral cavity within 0-120 seconds is ≥40%; the pouchable nicotine product can be stored at room temperature for at least 180 days.

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