Gas microcapsule, nicotine bag product and preparation method of nicotine bag product

Abstract

The invention discloses a gas microcapsule, a nicotine bag product and a preparation method thereof, the gas microcapsule is a three-dimensional mesh gel structure formed by a cross-linking reaction of a sodium alginate solution and a calcium chloride solution under the action of an emulsifier when CO2 gas is introduced, so that the CO2 gas is wrapped by the three-dimensional mesh gel structure. According to the preparation method, sodium alginate forms gas in water under the emulsification action of Tween 80, sodium alginate and a calcium chloride solution are chelated to form a three-dimensional mesh gel structure, CO2 is wrapped in a gel network, spherical gas microcapsules are prepared after drying, and nicotine bags are filled with the spherical gas microcapsules. When the nicotine bag is placed in the oral cavity to be eaten, the sound similar to'crisp 'can be generated, the eating interestingness of a user is increased, the adding content of the gas microcapsules can be accurately controlled, rapid release of nicotine is promoted, and meanwhile the production cost is greatly reduced.

Description

Technical Field

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

[0002] The way nicotine pouches are used is different from traditional cigarette inhalation. Nicotine pouches do not require burning or inhaling smoke. Instead, the small pouch containing nicotine is placed between the gums and lips, and the nicotine is absorbed directly through the oral mucosa. This avoids harmful substances such as tar and carbon monoxide produced by tobacco combustion. The process is smokeless and ashless, and it can be used discreetly in non-smoking areas without producing secondhand smoke, which makes it attractive to the public.

[0003] With increasing global attention to smoking and health issues, and intensifying tobacco control efforts, smokeless tobacco products are undoubtedly a viable alternative for smokers. In countries like the United States and Sweden, snuff and chewing tobacco have a long history, and the safety of nicotine mouthpieces has been validated by the market over a long period. Sweden and the United States are major global markets for nicotine mouthpieces. Both countries have a tradition of using smokeless products. In the United States, nicotine mouthpieces currently account for 2% of the tobacco market. In the US nicotine mouthpiece market, one brand stands out: ZYN from the Swedish match company. Launched in the US in 2016, the brand has seen continuous sales growth since its launch and has become a leader in the nicotine mouthpiece market. ZYN's market coverage is particularly high in the western United States, where it was first launched. In recent years, the UK and the Middle East have also seen explosive growth.

[0004] When regular nicotine products are ingested, the burning sensation of nicotine or a high pH level often causes a stinging sensation in the mouth, leading to an uncomfortable consumption experience. Currently, there are reports of oral nicotine products with a unique "popping" sensation. For example, patent document CN118749701A discloses a process for preparing oral cigarette filling particles that release carbon dioxide gas to accelerate nicotine release. This mainly involves adding popping candy particles to the nicotine pouch formula. The carbon dioxide gas contained in the popping candy particles accelerates the release of nicotine from the oral cigarette, making it easier for consumers to obtain nicotine. The popping candy absorbs water and melts in the mouth, instantly bursting and releasing gas, producing a "popping" sound. While this increases the fun of ingesting nicotine products and provides a unique taste and auditory experience, it is an added commercially available or homemade popping candy particle, and excessive sugar intake can pose health risks. The patent document with publication number CN104522873B discloses a soft mouthwash and its preparation method. By melting tobacco powder, sugar, binder, natural flavoring, flavoring agent and water and then pumping CO2 under high pressure, it can also produce a similar "crackling" sound to increase the fun. However, it is necessary to add corn starch or defatted soybean powder for molding, which increases the cost of preparing mouthwash.

[0005] Therefore, there is an urgent need to develop a nicotine pouch containing gas microcapsules that can produce a "crackling" sound when placed in the mouth, increasing the fun, precisely controlling the amount of gas microcapsules added, promoting the rapid release of nicotine, and reducing production costs. Summary of the Invention

[0006] The purpose of this patent is to provide a gas microcapsule, a nicotine pouch, and a method for preparing the same, so that when the nicotine pouch is placed in the mouth for consumption, it produces a "crackling" sound, increasing the fun, precisely controlling the amount of gas microcapsule added, promoting the rapid release of nicotine, and reducing production costs.

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

[0008] A gas microcapsule is a three-dimensional network gel structure formed by the cross-linking reaction of sodium alginate solution and calcium chloride solution under the action of an emulsifier when CO2 gas is introduced, so that the three-dimensional network gel structure can encapsulate CO2 gas.

[0009] Furthermore, the particle size of the gas microcapsules is 500~600 μm, 600~800 μm, 800~1000 μm or 1000~1200 μm.

[0010] Furthermore, the concentration of the sodium alginate solution is 1.0~1.5%, 1.5~2.0%, 2.0~2.5%, 2.5~3.0%, or 3.0~5.0%.

[0011] Furthermore, the concentration of the calcium chloride solution is 1.0~1.5%, 1.5~2.0%, 2.0~2.5%, 2.5~3.0%, or 3.0~5.0%.

[0012] Furthermore, the CO2 gas flow rate is 0.3~0.5 L / min, 0.5~0.6 L / min, or 0.6~0.8 L / min.

[0013] Another aspect of this patent provides a nicotine pouch product, which includes contents and outer packaging; the contents include the aforementioned gas microcapsules, and the amount of gas microcapsules added accounts for 10-20%, 20-40%, or 40-70% of the contents by mass.

[0014] This patent also provides a method for preparing a nicotine pouch product, including the following steps:

[0015] Step A: Add an emulsifier to the sodium alginate solution to prepare an emulsified sodium alginate solution; introduce CO2 gas into the emulsified sodium alginate solution and stir to prepare a bubble dispersion system;

[0016] Step B: The bubble dispersion system is added dropwise to the calcium chloride solution, and after standing, gel microspheres are obtained; the gel microspheres are rinsed with pure water and dried to obtain gas microcapsules;

[0017] Step C: Fill the contents of the nicotine pouch product with gas microcapsules, and then prepare the nicotine pouch product after outer packaging and ultraviolet sterilization.

[0018] Furthermore, in step A, the final concentration of the emulsifier in the emulsified sodium alginate solution is 0.1~0.2 mg / mL.

[0019] Furthermore, the CO2 gas was introduced under the following conditions: at a depth of 3-7 cm below the surface of the emulsified sodium alginate solution, the gas was introduced at a rate of 0.3-0.8 L / min, and magnetic stirring was performed. The temperature of the magnetic stirring was 25℃, the speed of the magnetic stirring was 800-1000 rpm, and the stirring time was 10-15 min.

[0020] Furthermore, in step B, the dropping rate of the bubble dispersion system is 1 drop / second.

[0021] Furthermore, the settling temperature is 25~28℃, and the settling time is 5~8 min, 8~12 min, or 12~15 min.

[0022] Furthermore, the drying temperature is 35~45℃, and the drying time is 10~16 h.

[0023] Furthermore, the particle size of the gel microspheres is 500~600 μm, 600~800 μm, 800~1000 μm or 1000~1200 μm.

[0024] Furthermore, in step C, the outer packaging includes nonwoven fabric, which includes medical-grade nonwoven fabric. The medical-grade nonwoven fabric is one or more combinations of polypropylene fiber, polyester fiber, polyamide fiber, polytetrafluoroethylene fiber, and glass fiber, and the basis weight of the nonwoven fabric is 25~35 g / m³. 2 .

[0025] The contents of the nicotine pouch, if chosen, also include a cellulose carrier, nicotine source, sweetener, pH adjuster, and flavorings. The cellulose carrier is used to adsorb the nicotine source, sweetener, pH adjuster, and flavorings.

[0026] The cellulose carrier is optionally a cellulose derivative, including one or more combinations of cellulose ethers, cellulose esters, or cellulose ether esters; the cellulose esters include cellulose nitrates, cellulose acetates, cellulose acetate butyrates, or cellulose xanthates; the cellulose ethers include methylcellulose, carboxymethylcellulose, ethylcellulose, hydroxyethylcellulose, cyanoethylcellulose, hydroxypropylcellulose, or hydroxypropylmethylcellulose.

[0027] The amount of nicotine source added is 1%~3%, 3%~5%, 5%~10%, 10%~12%, or 12%~15% of the weight of the cellulose carrier, and the nicotine loading in the nicotine source is 10~15%. The nicotine source includes nicotine salts or nicotine-ion exchange resins. 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. The ion exchange resin can be an acidic ion exchange resin, including strongly acidic cation exchange resins or weakly acidic cation exchange resins. The strongly acidic cation exchange resin includes one or more combinations of styrene strongly acidic ion exchange resins and macroporous strongly acidic ion exchange resins. The weakly acidic cation exchange resin includes one or more combinations of isobutyrate ion exchange resins, acrylic acid ion exchange resins, and 724 weakly acidic ion exchange resins.

[0028] The amount of sweetener added is optional, ranging from 3% to 6%. The sweetener includes one or more combinations of sucrose, saccharin, sucralose, glucose, maltose, corn syrup, cyclamate, aspartame, acesulfame potassium, xylitol, mannose, salts of acesulfame (e.g., potassium acesulfame), alitame, cyclohexanesulfonic acid and its salts, glycyrrhizin, dihydrochalcone, kiwifruit protein, indigofera protein, and stevioside.

[0029] The pH adjuster can be selected at a dosage of 0.1-0.5%. The pH adjuster includes one or more combinations of malic acid, citric acid, trisodium citrate, potassium citrate, acetic acid, adipic acid, fumaric acid, gluconic acid-δ-lactone, gluconic acid, lactic acid, maleic acid, tartaric acid, succinic acid, propionic acid, ascorbic acid, phosphoric acid, sodium orthophosphate, potassium orthophosphate, calcium orthophosphate, sodium diphosphate, potassium diphosphate, calcium diphosphate, pentasodium triphosphate, pentapotassium triphosphate, sodium polyphosphate, and potassium polyphosphate.

[0030] Optionally, the added flavorings are 0.5% to 2.0%, including coconut, coffee, chocolate, vanilla, citrus (e.g., grapefruit, orange, lime, bergamot, or lemon), menthol, licorice, caramel, honey, peanut, walnut, cashew, hazelnut, almond, pineapple, strawberry, raspberry, tropical fruit, 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 flavor, bergamot, and plum). Preferably, the flavorings also contain 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.

[0031] As an option, nicotine pouch products also include preservatives, including one or more combinations of potassium sorbate, benzoic acid, sodium benzoate, and sorbic acid.

[0032] The size of any nicotine oral product is 0.8–0.9 cm. 3 0.9~1.2 cm 3 Or 1.2~1.4 cm 3 .

[0033] The outer packaging may also include flavorings and fragrances for added aroma.

[0034] As used in this patent, "nicotine pouch" generally refers to a smokeless oral tobacco product that is placed between the lips and gums during use and allows some of the soluble substances to dissolve through saliva.

[0035] 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.

[0036] This patent provides a gas microcapsule, nicotine pouch, and their preparation method. The method involves forming a gas-in-water mixture using sodium alginate emulsified at Tween 80, followed by chelation between sodium alginate and calcium chloride solution to create a three-dimensional network gel structure that encapsulates CO2 within the gel network. After drying, spherical gas microcapsules are prepared and filled into nicotine pouches. When the nicotine pouch is placed in the mouth, it produces a crackling sound, increasing the user's enjoyment. The method allows for precise control of the added gas microcapsule content, promoting rapid nicotine release while significantly reducing production costs. Attached Figure Description

[0037] 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.

[0038] Figure 1 This is a flowchart illustrating the preparation process of the nicotine bag in this patent embodiment. Detailed Implementation

[0039] 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.

[0040] In this specification and claims, several terms will be used, and unless otherwise indicated, these terms will be defined to have the following meanings:

[0041] As used in this patent, "TGA" stands for thermogravimetric analysis, a thermal analysis technique that measures the relationship between the mass of a sample and temperature change under programmed temperature control. When the analyte undergoes sublimation, vaporization, decomposition into gas, or loss of water of crystallization during heating, its mass changes. In this case, the thermogravimetric curve is no longer a straight line but rather shows a decrease. By analyzing the thermogravimetric curve, one can determine at what temperature the analyte undergoes this change, and based on the weight loss, calculate how much substance has been lost.

[0042] 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.

[0043] All other terms used herein for special definition are intended to have the general meaning understood by one of ordinary skill in the art, and 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.

[0044] 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.

[0045] 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.

[0046] Unless otherwise specified, all embodiments and preferred embodiments mentioned herein can be combined to form new technical solutions.

[0047] Unless otherwise specified, all the technical features and preferred features mentioned herein can be combined to form new technical solutions.

[0048] 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 method may also include step (c), indicating 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.

[0049] 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.

[0050] 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.

[0051] 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).

[0052] Unless otherwise specified, percentages (%) in this document refer to percentages by mass relative to the composition.

[0053] Unless otherwise stated herein, the sum of the contents of the components in the composition is 100%.

[0054] 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.

[0055] Unless otherwise specified, the term "a" as used in this specification means "at least one".

[0056] 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.

[0057] 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.

[0058] 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.

[0059] like Figure 1 As shown, this patent provides a gas microcapsule, a nicotine pouch product, and a method for preparing the same, comprising the following steps:

[0060] S1. Preparation of sodium alginate solution, the specific steps are as follows:

[0061] (1) Weigh 1.0~5.0 g of sodium alginate (commercially available, analytical grade, viscosity 350 mPa·s), add 95.0~99.0 mL of distilled water, and stir in a water bath at 55~65℃ until completely dissolved to obtain a sodium alginate solution with a concentration of 1.0~5.0%.

[0062] The stirring speed is 100~400 rpm, and the stirring time is 5~25 minutes, so that the sodium alginate can be completely dissolved in the water.

[0063] (2) Add Tween 80 (commercially available, nonionic surfactant) to the sodium alginate solution prepared in step (1) above, so that the final concentration of Tween 80 is 0.1~0.2 mg / mL, and stir evenly to obtain the emulsified sodium alginate solution.

[0064] S2. Preparation of the bubble dispersion system, the specific steps are as follows:

[0065] The conduit is inserted 3-7 cm below the surface of the emulsified sodium alginate solution prepared in step S1 (2) above, and CO2 gas is injected at a flow rate of 0.3-0.8 L / min. The mixture is then stirred using a commercially available magnetic stirrer to form a uniform bubble dispersion system. At this point, the bubble dispersion system is a water-in-gas (W / G) dispersion, i.e., a sodium alginate solution containing bubbles, wherein the diameter of the bubbles is 50-200 μm.

[0066] The stirring conditions for the magnetic stirrer are: at 25℃, the speed is set to 800~1000 rpm, and stirring is carried out for 10~15 minutes.

[0067] S3. Preparation of CO2 gas microcapsules, the specific steps are as follows:

[0068] (1) Preparation of calcium chloride solution: Weigh 1~5 g of calcium chloride (commercially available, analytical grade), add it to 95~99 mL of distilled water, stir until completely dissolved, and obtain a calcium chloride solution with a concentration of 1.0~5.0%.

[0069] (2) Using a syringe (commercially available), extract the sodium alginate solution containing bubbles prepared in step S2 above, keep the needle of the syringe 10 cm above the surface of the calcium chloride solution with a concentration of 1.0~5.0% prepared above, and drop the sodium alginate solution containing bubbles into the calcium chloride solution.

[0070] The sodium alginate solution containing air bubbles is added at a rate of 1 drop / second and allowed to stand at room temperature (25-28℃) for 5-15 minutes. This allows the carboxyl groups in the sodium alginate to chelate with the calcium ions in the calcium chloride solution, forming a three-dimensional network gel structure (also known as an egg-box model). This encapsulates CO2 gas within the gel network, forming gel microspheres with a particle size of 500-1200 μm. The cross-linking time is 5-15 minutes to ensure the gel network is fully densified, forming a semi-permeable wall material to prevent CO2 gas escape.

[0071] Alternatively, a microfluidic device can be used to replace the syringe, allowing for more precise control of the gel microsphere particle size, for example, controlling the particle size of the gel microsphere to 600±50 μm.

[0072] (3) Collect the gel microspheres prepared in step (2) using a mesh sieve with a pore size of 500~1000 μm, and repeatedly rinse the gel microspheres with distilled water to remove residual calcium chloride.

[0073] (4) Place the gel microspheres that have been repeatedly rinsed in step (3) above into an oven to dry. The drying conditions are 35~45℃ for 10~16 h. The dried gel microspheres are gas microcapsules.

[0074] S4. Prepare the nicotine pouch, the specific steps of which are as follows:

[0075] The gas microcapsules prepared in step S3 above are filled into the contents of the nicotine bag. The weight percentage of the gas microcapsules added is 10-20%, 20-40%, or 40-70% of the contents. After outer packaging and ultraviolet sterilization, the nicotine bag is prepared.

[0076] The contents of the nicotine pouch also include a cellulose carrier, nicotine source, sweetener, pH adjuster, and flavoring. The cellulose carrier is used to adsorb the nicotine source, sweetener, pH adjuster, and flavoring.

[0077] The cellulose carrier is a cellulose derivative, including one or more combinations of cellulose ethers, cellulose esters, or cellulose ether esters; the cellulose esters include cellulose nitrates, cellulose acetates, cellulose acetate butyrates, or cellulose xanthates; the cellulose ethers include methylcellulose, carboxymethylcellulose, ethylcellulose, hydroxyethylcellulose, cyanoethylcellulose, hydroxypropylcellulose, or hydroxypropylmethylcellulose.

[0078] The amount of nicotine source added is 1%~3%, 3%~5%, 5%~10%, 10%~12%, or 12%~15% of the weight of the cellulose carrier. The nicotine loading in the nicotine source is 10~15%. The nicotine source includes nicotine salts or nicotine-ion exchange resins. 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. The ion exchange resin can be an acidic ion exchange resin, including strongly acidic cation exchange resins or weakly acidic cation exchange resins. The strongly acidic cation exchange resin includes one or more combinations of styrene strongly acidic ion exchange resins and macroporous strongly acidic ion exchange resins. The weakly acidic cation exchange resin includes one or more combinations of isobutyrate ion exchange resins, acrylic acid ion exchange resins, and 724 weakly acidic ion exchange resins.

[0079] The amount of sweetener added is 3-6%, and the sweetener includes one or more combinations of sucrose, saccharin, sucralose, glucose, maltose, corn syrup, cyclamate, aspartame, acesulfame potassium, xylitol, mannose, salts of acesulfame (e.g., potassium acesulfame), alitame, cyclohexanesulfonic acid and its salts, glycyrrhizin, dihydrochalcone, kiwifruit protein, indigofera protein, and stevioside.

[0080] The pH adjuster is added at a rate of 0.1-0.5%, and includes one or more combinations of malic acid, citric acid, trisodium citrate, potassium citrate, acetic acid, adipic acid, fumaric acid, gluconic acid-δ-lactone, gluconic acid, lactic acid, maleic acid, tartaric acid, succinic acid, propionic acid, ascorbic acid, phosphoric acid, sodium orthophosphate, potassium orthophosphate, calcium orthophosphate, sodium diphosphate, potassium diphosphate, calcium diphosphate, pentasodium triphosphate, pentapotassium triphosphate, sodium polyphosphate, and potassium polyphosphate.

[0081] The amount of flavoring added is 0.5-2.0%, and the flavoring includes coconut, coffee, chocolate, vanilla, citrus (e.g., grapefruit, orange, lime, bergamot, or lemon), menthol, licorice, caramel, honey, peanut, walnut, cashew, hazelnut, almond, pineapple, strawberry, raspberry, tropical fruit, 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 flavoring also contains 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.

[0082] Example 1

[0083] (1) Weigh 1.5 g of sodium alginate, add 98.5 mL of distilled water, and place it in a 60℃ water bath and stir until completely dissolved. The stirring speed is 200 rpm and the stirring time is 10 min to obtain a first solution with a concentration of 1.5%.

[0084] (2) Add Tween 80 to the first solution prepared in step (1) above so that the final concentration of Tween 80 is 0.1 mg / mL, stir evenly to obtain the second solution, which is sodium alginate solution.

[0085] (3) Insert the conduit into the sodium alginate solution prepared in step (2) above 5 cm below the liquid surface, and inject CO2 gas at a flow rate of 0.5 L / min. At 25°C, stir with a magnetic stirrer at a speed of 1000 rpm for 10 min to form a uniform bubble dispersion system.

[0086] (4) Weigh 2 g of calcium chloride, add it to 98 mL of distilled water, and stir until completely dissolved to obtain a calcium chloride solution with a concentration of 2.0%.

[0087] (5) Use a syringe to extract the sodium alginate solution containing bubbles prepared in step (3) above. Keep the needle of the syringe 10 cm above the surface of the calcium chloride solution with a concentration of 2.0% prepared in step (4) above. Add the sodium alginate solution containing bubbles to the calcium chloride solution at a dropping rate of 1 drop / second and let it stand at room temperature for 5 min to obtain gel microspheres.

[0088] (6) Collect the gel microspheres prepared in step (5) using a mesh sieve with a pore size of 500 μm, and rinse the gel microspheres three times with distilled water to remove residual calcium chloride.

[0089] (7) Place the gel microspheres that have been repeatedly rinsed in step (6) above in an oven to dry. The drying conditions are 40°C for 12 h. The dried gel microspheres are gas microcapsules.

[0090] (8) The gas microcapsules prepared in step (7) above are filled into the contents of the nicotine bag. The weight percentage of the gas microcapsules added is 10% of the contents. After outer packaging and ultraviolet sterilization, the nicotine bag is prepared.

[0091] Example 2

[0092] (1) Weigh 2.0 g of sodium alginate, add 98.0 mL of distilled water, and place it in a 60℃ water bath and stir until completely dissolved. The stirring speed is 200 rpm and the stirring time is 15 min to obtain a first solution with a concentration of 2.0%.

[0093] (2) Add Tween 80 to the first solution prepared in step (1) above so that the final concentration of Tween 80 is 0.1 mg / mL, stir evenly to obtain the second solution, which is sodium alginate solution.

[0094] (3) Insert the conduit into the sodium alginate solution prepared in step (2) above 5 cm below the liquid surface, and inject CO2 gas at a flow rate of 0.5 L / min. At 25°C, stir with a magnetic stirrer at a speed of 1000 rpm for 10 min to form a uniform bubble dispersion system.

[0095] (4) Weigh 2 g of calcium chloride, add it to 98 mL of distilled water, and stir until completely dissolved to obtain a calcium chloride solution with a concentration of 2.0%.

[0096] (5) Use a syringe to draw the sodium alginate solution containing bubbles prepared in step (3) above, keep the needle of the syringe 10 cm above the surface of the calcium chloride solution with a concentration of 2.0% prepared in step (4) above, add the sodium alginate solution containing bubbles to the calcium chloride solution at a dropping rate of 1 drop / second, and let it stand at room temperature for 10 min to obtain gel microspheres;

[0097] (6) Collect the gel microspheres prepared in step (5) using a mesh sieve with a pore size of 500 μm, and rinse the gel microspheres three times with distilled water to remove residual calcium chloride.

[0098] (7) Place the gel microspheres that have been repeatedly rinsed in step (6) above in an oven to dry. The drying conditions are 40°C for 12 h. The dried gel microspheres are gas microcapsules.

[0099] (8) The gas microcapsules prepared in step (7) above are filled into the contents of the nicotine bag. The weight percentage of the gas microcapsules added is 30% of the contents. After outer packaging and ultraviolet sterilization, the nicotine bag is prepared.

[0100] Example 3

[0101] (1) Weigh 2.5 g of sodium alginate, add 97.5 mL of distilled water, and place it in a 60℃ water bath and stir until completely dissolved. The stirring speed is 300 rpm and the stirring time is 10 min to obtain a first solution with a concentration of 2.5%.

[0102] (2) Add Tween 80 to the first solution prepared in step (1) above so that the final concentration of Tween 80 is 0.1 mg / mL, stir evenly to obtain the second solution, which is sodium alginate solution.

[0103] (3) Insert the conduit into the sodium alginate solution prepared in step (2) above 5 cm below the liquid surface, and inject CO2 gas at a flow rate of 0.5 L / min. At 25°C, stir with a magnetic stirrer at a speed of 1000 rpm for 10 min to form a uniform bubble dispersion system.

[0104] (4) Weigh 2 g of calcium chloride, add it to 98 mL of distilled water, and stir until completely dissolved to obtain a calcium chloride solution with a concentration of 2.0%.

[0105] (5) Use a syringe to draw the sodium alginate solution containing bubbles prepared in step (3) above, keep the needle of the syringe 10 cm above the surface of the calcium chloride solution with a concentration of 2.0% prepared in step (4) above, add the sodium alginate solution containing bubbles to the calcium chloride solution at a dropping rate of 1 drop / second, and let it stand at room temperature for 15 min to obtain gel microspheres;

[0106] (6) Collect the gel microspheres prepared in step (5) using a mesh sieve with a pore size of 500 μm, and rinse the gel microspheres three times with distilled water to remove residual calcium chloride.

[0107] (7) Place the gel microspheres that have been repeatedly rinsed in step (6) above in an oven to dry. The drying conditions are 40°C for 12 h. The dried gel microspheres are gas microcapsules.

[0108] (8) The gas microcapsules prepared in step (7) above are filled into the contents of the nicotine bag. The weight percentage of the gas microcapsules added is 50% of the contents. After outer packaging and ultraviolet sterilization, the nicotine bag is prepared.

[0109] Comparative Example 1

[0110] 0.5g of commercially available ZYN brand nicotine bag powder was weighed out as the contents of the nicotine bag, sealed in a non-woven fabric outer packaging, and sterilized with ultraviolet light to prepare the nicotine bag.

[0111] Comparative Example 2

[0112] Nicotine bags were prepared using the preparation method disclosed in Chinese patent document CN104522873B.

[0113] Test Example 1: Detection of Physical Properties of Gas Microcapsules

[0114] To illustrate the advantages of this patent, the average diameter, CO2 retention rate (TGA), and dissolution time in pure water of the gas microcapsules prepared in Examples 1-3 were measured using existing instruments and equipment.

[0115] The results are shown in Table 1. With increasing sodium alginate concentration, the particle size of the gas microcapsules gradually decreased. The increased viscosity of the sodium alginate solution inhibited bubble coalescence, leading to improved CO2 retention. A denser gel network structure was formed in the high-concentration sodium alginate solution, and the CO2 release rate was faster in pure water. Simultaneously, extending the cross-linking time from 5 min to 15 min increased the CO2 retention rate from 72.3% to 91.2%, due to the increased Ca... 2+The cross-linking is more complete, but after more than 10 minutes of cross-linking, the dissolution time does not improve significantly, possibly because excessive hardening of the wall material hinders rapid cracking.

[0116] In Example 1, the average diameter of the gas microcapsules prepared was 1000±150 μm, the CO2 retention rate was 72.3%, and the dissolution time of the gas microcapsules in pure water was 8.2 s; in Example 2, the average diameter of the gas microcapsules prepared was 850±80 μm, the CO2 retention rate was 88.5%, and the dissolution time of the gas microcapsules in pure water was 5.5 s; in Example 3, the average diameter of the gas microcapsules prepared was 650±50 μm, the CO2 retention rate was 91.2%, and the dissolution time of the gas microcapsules in pure water was 4.1 s.

[0117] Table 1. Physical properties of the gas microcapsules prepared in Examples 1-3

[0118] Example 1 Example 2 Example 3 Sodium alginate concentration 1.5% 2.0% 2.5% Crosslinking time (min) 5 10 15 Average diameter of microcapsules (μm) 1000±150 850±80 600±50 <![CDATA[CO2 retention rate (TGA)]]> 72.3% 88.5% 91.2% Dissolution time (s) 8.2 5.5 4.1

[0119] Test Example 2: Taste Test of Nicotine Bags

[0120] To further illustrate the advantages of this patent, taste tests were conducted on the nicotine bags prepared in Examples 1-3 and Comparative Examples 1-2. The preparation method of the nicotine bags in Examples 1-3 was as follows: 50 parts by weight of each of the gas microcapsules prepared in Examples 1-3 were weighed and mixed with 50 parts of commercially available ZYN brand nicotine bag powder. After mixing evenly, 0.5 g was weighed as the contents, packaged in a non-woven fabric outer packaging, and sterilized with ultraviolet light to obtain the nicotine bag.

[0121] The taste test method is as follows: a professional evaluation team (n=7) will conduct the evaluation, and the above-mentioned mouthwash will be placed directly between the upper lip and the upper teeth. The standard consumption time is set at 5 minutes.

[0122] The scoring criteria are as follows:

[0123] A 10-point scale is used, with 1 point being extremely weak / none and 10 points being extremely strong.

[0124] The results are shown in Table 2. The nicotine pouches prepared by the methods described in Examples 1-3 exhibited a "jumping sensation" in the oral cavity, demonstrating good performance. The nicotine quickly reached the head within 40 seconds, with a moderate strength and a slightly gradual duration of the strength. In contrast, Comparative Example 1 failed to produce a "jumping sensation," and the nicotine began to reach the head around 1 minute later, but the strength of the strength was high at the beginning and low at the end, resulting in a poor experience. Comparative Example 2, while exhibiting a "jumping sensation" in the oral cavity and demonstrating good performance, also began to reach the head around 1 minute later, with a moderate strength and a strong duration of the strength.

[0125] Table 2 Taste rating table for nicotine pouches in Examples 1-3 and Comparative Examples 1-2

[0126] Serial Number Finished product's dynamic performance Jumping feel (out of 10) nicotine uptake duration Example 1 It has a "jumping" sensation in the mouth and performs well. 9.2 It takes about 30 seconds to get the kick in, the intensity is moderate, and the feeling of invigoration lasts for a relatively long time. Example 2 It has a "jumping" sensation in the mouth and performs well. 9.4 It takes about 40 seconds to get the kick in, the intensity is moderate, and the feeling of invigoration lasts for a relatively short time. Example 3 It has a distinct "jumping" sensation in the oral cavity and excellent performance. 9.5 It takes about 40 seconds to get the kick in, the intensity is moderate, and the feeling of invigoration lasts for a relatively short time. Comparative Example 1 Unable to create a "jumping" feeling / On average, the effects begin to kick in after 1 minute, with a strong initial surge that lasts longer before waning. Comparative Example 2 It has a "jumping" sensation in the mouth and performs well. 9.2 On average, the effects begin to kick in after about 1 minute, but the intensity is moderate, and the duration of the effect is high at the beginning and low at the end.

[0127] Therefore, it can be concluded that the gas microcapsules, nicotine pouches, and their preparation method provided by this patent utilize sodium alginate emulsified at Tween 80 to form a water-in-gas mixture. The CO2 is then encapsulated within the gel network through chelation between sodium alginate and calcium chloride solution. After drying, spherical gas microcapsules are prepared and filled into nicotine pouches. When the nicotine pouch is placed in the mouth, it produces a crackling sound, increasing the user's enjoyment. The addition of gas microcapsules allows for precise control of the amount added, promoting rapid nicotine release while significantly reducing production costs.

[0128] 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.

[0129] 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.

[0130] 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.

[0131] 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 gas microcapsule, characterized in that, The gas microcapsules are three-dimensional network gel structures formed by the cross-linking reaction of sodium alginate solution and calcium chloride solution under the action of an emulsifier when CO2 gas is introduced, so that the three-dimensional network gel structure can encapsulate the CO2 gas.

2. The gas microcapsule according to claim 1, characterized in that, The gas microcapsules have a particle size of 500~600μm, 600~800μm, 800~1000μm or 1000~1200μm.

3. The gas microcapsule according to claim 1, characterized in that, The concentration of the sodium alginate solution is 1.0~1.5%, 1.5~2.0%, 2.0~2.5%, 2.5~3.0%, or 3.0~5.0%. The concentration of the calcium chloride solution is 1.0~1.5%, 1.5~2.0%, 2.0~2.5%, 2.5~3.0%, or 3.0~5.0%.

4. The gas microcapsule according to claim 1, characterized in that, The CO2 gas flow rate is 0.3~0.5 L / min, 0.5~0.6 L / min, or 0.6~0.8 L / min.

5. A nicotine pouch product, characterized in that, The nicotine pouch product includes the contents and the outer packaging; The contents include gas microcapsules as described in any one of claims 1 to 4, wherein the amount of gas microcapsules added is 10 to 20%, 20 to 40%, or 40 to 70% of the contents by mass.

6. A method for preparing the nicotine pouch product according to claim 5, characterized in that, Includes the following steps: Step A: Add an emulsifier to the sodium alginate solution to prepare an emulsified sodium alginate solution; CO2 gas was introduced into the emulsified sodium alginate solution, and the mixture was stirred to prepare a bubble dispersion system. Step B: The bubble dispersion system is added dropwise to the calcium chloride solution, and after standing, gel microspheres are obtained; the gel microspheres are rinsed with pure water and dried to obtain the gas microcapsules; Step C: The gas microcapsules are filled into the contents of the nicotine pouch product, and the nicotine pouch product is prepared after outer packaging and ultraviolet sterilization.

7. The method for preparing the nicotine pouch product according to claim 6, characterized in that, In step A The final concentration of the emulsifier in the emulsified sodium alginate solution is 0.1~0.2 mg / mL; The CO2 gas is introduced under the following conditions: at a depth of 3-7 cm below the surface of the emulsified sodium alginate solution, it is introduced at a rate of 0.3-0.8 L / min, while magnetic stirring is performed. The temperature of the magnetic stirring is 25°C, the speed of the magnetic stirring is 800-1000 rpm, and the stirring time is 10-15 min.

8. The method for preparing the nicotine pouch product according to claim 6, characterized in that, In step B, The dropping rate of the bubble dispersion system is 1 drop / second; The settling temperature is 25~28℃, and the settling time is 5~8 min, 8~12 min, or 12~15 min; The drying temperature is 35~45℃, and the drying time is 10~16 h.

9. The method for preparing the nicotine pouch product according to claim 8, characterized in that, The particle size of the gel microspheres is 500~600 μm, 600~800 μm, 800~1000 μm or 1000~1200 μm.

10. The method for preparing the nicotine pouch product according to claim 6, characterized in that, In step C, the outer packaging includes a nonwoven fabric, which includes a medical-grade nonwoven fabric. The medical-grade nonwoven fabric is one or more combinations of polypropylene fiber, polyester fiber, polyamide fiber, polytetrafluoroethylene fiber, and glass fiber, and the basis weight of the nonwoven fabric is 25-35 g / m³. 2 .

Images