Nicotine bagged product and preparation method thereof

Abstract

The invention discloses a nicotine bagged product and a preparation method thereof, the nicotine bagged product comprises a content and an outer package, and the content comprises a nicotine source; the outer package is prepared by adsorbing a nicotine source by a non-woven fabric under the action of a deep-eutectic solvent. According to the preparation method provided by the invention, a small amount of carboxyl groups are introduced to the surface of the non-woven fabric through the deep-eutectic solvent, so that the adsorption performance of the non-woven fabric to nicotine is remarkably improved, and the nicotine source and other additives such as the pH regulator are mixed to prepare the content; and placing the content in a modified non-woven fabric material, and carrying out shearing, hot pressing and ultraviolet sterilization to obtain the nicotine bagged product. The release efficiency of the nicotine bagged product in the oral cavity in the 10th minute is greater than or equal to 45.0%, and the release efficiency in the 40th minute is greater than or equal to 85.0%, so that a certain amount of nicotine can be released when the non-woven fabric is not soaked by saliva in the early stage in the use process of a consumer, and the defect that the nicotine release and delivery effects in the early stage are not obvious is overcome.

Description

Technical Field

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

[0002] Traditional tobacco products deliver nicotine through heated combustion, but this process generates a large amount of harmful substances such as tar and carbon monoxide, posing a serious threat to the health of smokers and those around them. Nicotine mouthwash differs from traditional cigarettes in that it does not require combustion or inhalation of smoke. Instead, the nicotine-containing oral product is placed between the gums and lips, allowing for direct absorption of nicotine through the oral mucosa. This avoids the harmful substances such as tar and carbon monoxide produced by tobacco combustion. It produces no smoke or ash, can be used discreetly in non-smoking areas, and does not generate secondhand smoke, making it attractive to the public.

[0003] Currently, nicotine used in novel nicotine products is mostly in the form of nicotine extracts, free nicotine, and liquid nicotine salts. These products utilize materials such as microcrystalline cellulose to adsorb nicotine and are often packaged in pouches. However, the outer packaging pouches themselves have limited adsorption capacity and function, failing to effectively adsorb and stably release nicotine. Furthermore, the nicotine contained within the pouches is often in a single form, primarily simple nicotine salt particles, making precise control of nicotine release and stability difficult. For example, patent document CN103491958A discloses a pouch containing nicotine in the form of free salts. By placing the free salts in a water-insoluble but saliva-permeable pouch, a pH adjuster allows the nicotine to be converted into free nicotine in the oral cavity for absorption. Although it achieves nicotine delivery to some extent, the material and internal structure of the pouch are relatively simple. It needs to be completely soaked in non-woven fabric before it can release nicotine after contacting the nicotine salt wrapped in the non-woven fabric. In the in vitro test, the nicotine release rate was only 41% at 16 minutes. Its absorption and release performance of nicotine is limited, and it cannot achieve rapid and continuous release.

[0004] Therefore, there is an urgent need to develop an oral nicotine pouch product that allows consumers to release a certain amount of nicotine even before their saliva has fully soaked the non-woven fabric during the initial use of the product. This would compensate for the shortcomings of oral nicotine pouch products, which have an unclear nicotine release and delivery effect in the early stages of use, reduce oral irritation, provide richer flavor characteristics, reduce production costs, and enhance the consumer experience. Summary of the Invention

[0005] The purpose of this patent is to provide an oral nicotine pouch product and its preparation method, so that a certain amount of nicotine can be released even when the saliva has not yet soaked the non-woven fabric during the initial use of the nicotine pouch product. This is intended to make up for the shortcoming of the unclear nicotine release and delivery effect in the early stage of use of oral nicotine pouch products, reduce oral irritation, provide richer flavor characteristics, reduce production costs, and enhance the consumer experience.

[0006] To solve the above-mentioned technical problems, this patent adopts the following technical solution:

[0007] This patent provides a nicotine pouch product, which includes contents and outer packaging.

[0008] The contents include nicotine sources;

[0009] The outer packaging is prepared by adsorbing nicotine source onto nonwoven fabric under the action of a eutectic solvent.

[0010] Furthermore, the nonwoven fabric is immersed in a eutectic solvent, which allows carboxyl groups to be attached to the nonwoven fabric.

[0011] Furthermore, the soaking temperature is 50~55℃, 55~65℃, or 65~70℃.

[0012] Furthermore, the soaking time is 2-3 hours, 3-4 hours, or 4-5 hours.

[0013] Furthermore, the eutectic solvent includes hydrogen bond acceptors and hydrogen bond donors, with a molar ratio of hydrogen bond acceptors to hydrogen bond donors of 1:(1~4).

[0014] Furthermore, hydrogen bond acceptor reagents include quaternary ammonium salts and / or zwitterions; quaternary ammonium salts include choline chloride, and zwitterions include betaine.

[0015] Furthermore, hydrogen bond donors include one or more combinations of urea, thiourea, carboxylic acids, polyols, amino acids, sugars, and trifluoroacetamide.

[0016] Furthermore, carboxylic acids include one or more combinations of phenylacetic acid, malic acid, citric acid, and succinic acid; polyols include one or more combinations of ethylene glycol, glycerol, butanediol, and xylitol; and sugars include glucose and / or fructose.

[0017] Furthermore, the nicotine source includes one or more combinations of free nicotine, nicotine salts, nicotine-ion exchange resins, nicotine complexes, and non-covalently bound nicotine.

[0018] 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.

[0019] Furthermore, the concentration of the nicotine source is 50-80 mg / mL, 80-100 mg / mL, or 100-150 mg / mL.

[0020] Furthermore, the adsorption temperature of nonwoven fabrics in nicotine sources is 24~25℃, 25~27℃, or 27~30℃.

[0021] Furthermore, the adsorption time of nonwoven fabrics in nicotine sources is 1.0~1.5 h, 1.5~2.0 h, or 2.0~3.0 h.

[0022] Furthermore, the contents also include a pH adjuster, with the nicotine source and pH adjuster mixed to form particulate contents.

[0023] Furthermore,

[0024] Furthermore, the size of the nicotine pouch product is (1.2~2.5)×(1.5~3.0) cm;

[0025] Furthermore, the weight of the nicotine pouch products is 0.3~0.4 g, 0.4~0.6 g, 0.6~0.8 g, or 0.8~0.9 g.

[0026] Furthermore, the nicotine pouch product exhibits a release efficiency of ≥45.0% in the oral cavity from minute 0 to minute 10;

[0027] Furthermore, the nicotine pouch product has a release efficiency of ≥85.0% in the oral cavity from 0 to 40 minutes.

[0028] This patent also provides a method for preparing a nicotine pouch product, including the following steps:

[0029] Step A: Pre-treat the nonwoven fabric in a eutectic solvent to obtain a nonwoven fabric containing carboxyl groups;

[0030] Step B: Place the nonwoven fabric containing carboxyl groups in a nicotine source for adsorption to obtain a nonwoven fabric containing nicotine;

[0031] Step C: Mix the nicotine source with the additives to obtain the contents, place the contents in a non-woven fabric containing nicotine, and obtain the nicotine bagged product after shearing, hot pressing and ultraviolet sterilization.

[0032] Furthermore, in step A, the pretreatment conditions are heating and stirring.

[0033] Furthermore, the heating and stirring temperature is 80~95℃, and the heating and stirring time is 10~40 min.

[0034] Furthermore, in step B, the adsorption temperature is 24~28℃.

[0035] Furthermore, the adsorption time is 1~2 h or 2~3 h.

[0036] Furthermore, in step B, the adsorption temperature is 24~30℃, and the adsorption time is 1.0~1.5 h, 1.5~2.0 h, or 2.0~3.0 h.

[0037] Furthermore, in step C, the amount of additive added is 2.0 to 8.0% of the weight ratio of nicotine source, and the nicotine loading in the nicotine source is 1.0 to 1.5 mg, 1.5 to 2.0 mg, or 2.0 to 3.0 mg.

[0038] Furthermore, nonwoven fabrics containing nicotine are single-layer or double-layer nonwoven fabrics.

[0039] Furthermore, the double-layer nonwoven fabric is specifically designed such that the amount of nicotine source adsorbed at the end closer to the contents is less than the amount of nicotine source adsorbed at the end farther from the contents.

[0040] Furthermore, the additives include pH adjusters, with the amount of pH adjusters added being 1.0 to 5.0% of the weight ratio of the nicotine source.

[0041] Furthermore, the pH adjuster is selected from acetic acid, adipic acid, citric acid, fumaric acid, gluconic acid-δ-lactone, gluconic acid, lactic acid, malic 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, potassium polyphosphate, carbonic acid, sodium carbonate, sodium bicarbonate, potassium carbonate, calcium carbonate, magnesium carbonate, magnesium oxide, metal hydroxides, or any combination thereof.

[0042] In an advantageous embodiment of the invention, the additive further includes flavorings, wherein the amount of flavorings added is 2.0 to 5.0% of the weight ratio of the nicotine source.

[0043] Further, non-exhaustive examples of flavorings include coconut, coffee, chocolate, vanilla, citrus fruits (e.g., grapefruit, orange, lime, bergamot, or lemon), menthol, licorice, caramel, honey, peanut, walnut, cashew, hazelnut, almond, pineapple, strawberry, raspberry, tropical fruits, cherry, cinnamon, peppermint, deer antler, spearmint, eucalyptus, mint, and fruit flavorings (e.g., flavorings from apple, pear, peach, strawberry, apricot, raspberry, cherry, pineapple, lemongrass, lime, chili (capsaicin), citrus, tobacco flavor, bergamot, and plum). Preferably, the flavorings also contain essential oils, including peppermint, spearmint, menthol, eucalyptus, clove oil, laurel oil, fennel, thyme, cedarwood oil, nutmeg, and oils from the aforementioned fruits.

[0044] In an advantageous embodiment of the invention, the additive further includes a cooling agent, the amount of which is 0.3 to 1.0% of the weight ratio of the nicotine source.

[0045] Further, non-exhaustive examples of cooling agents include menthol, peppermint extract, or WS-23 (a commercially available cooling agent).

[0046] In an advantageous embodiment of the invention, the additive further includes a sweetener, the amount of which is 1.0 to 5.0% of the weight ratio of the nicotine source.

[0047] Further, non-exhaustive examples of sweeteners include one or more combinations of white sugar, glucose, maltose, corn syrup, lactose, cyclamate, xylitol, aspartame, acesulfame potassium, saccharin, sucralose, mannose, and erythritol; sucrose, sucralose, aspartame, salts of acesulfame (e.g., potassium acesulfame), alitame, saccharin and its salts, cyclohexanesulfonic acid and its salts, glycyrrhizin, dihydrochalcone, kiwifruit protein, indigofera protein, steviol glycosides, etc.

[0048] This patent provides a nicotine pouch product and its preparation method. A small amount of carboxyl groups are introduced onto the surface of a nonwoven fabric using a eutectic solvent, significantly improving the nonwoven fabric's adsorption performance for nicotine. The nicotine source is mixed with pH adjusters and other additives to prepare the contents. Then, using traditional processes, the contents are placed in a modified nonwoven fabric material, and the product is prepared by shearing, hot pressing, and ultraviolet sterilization. This results in a nicotine pouch product with a release efficiency of ≥45.0% from 0 to 10 minutes in the oral cavity and ≥85.0% from 0 to 40 minutes, achieving stable nicotine release and good nicotine delivery. This allows for the release of a certain amount of nicotine even before saliva has fully soaked the nonwoven fabric during the initial use of oral nicotine pouch products, compensating for the shortcomings of less effective nicotine release and delivery in the early stages of use. This reduces oral irritation while providing richer flavor characteristics, lowering production costs, and enhancing the consumer experience. Attached Figure Description

[0049] 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.

[0050] Figure 1 The graph shows the nicotine release curve in Test Example 1 of this patent (where the horizontal axis represents time in seconds and the vertical axis represents cumulative release in %). Detailed Implementation

[0051] 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.

[0052] In this specification and claims, several terms will be used, and unless otherwise indicated, these terms will be defined to have the following meanings:

[0053] As used in this patent, the term "free nicotine" (also known as nicotine) has the chemical formula C. 10 H 14 N2, a pyridine alkaloid, is found in tobacco and possesses certain physiological activities, used to provide tobacco flavor, etc. In this document, the terms "nicotine" and "nicotine" are used interchangeably. Free nicotine refers to the nicotine in a product that does not form any combination with any other components in the product during storage and before consumption by the consumer. Nicotine is provided by acting as a suitable salt; this nicotine source is non-volatile or not easily oxidized and is stable during storage.

[0054] As used in this patent, the term "nonwoven fabric" is also known as "non-woven cloth," which is a type of fabric formed without the need for weaving. It is made by arranging short textile fibers or filaments in a directional or random manner to form a web structure, which is then reinforced by mechanical, thermal bonding, or chemical methods.

[0055] As used in this patent, the term "DES solution (Deep Eutectic Solvent)," also known as a eutectic solvent, refers to a two- or three-component eutectic mixture composed of hydrogen bond acceptors (HBAs, such as quaternary ammonium salts) and hydrogen bond donors (HBDs, such as amides, carboxylic acids, and polyols) in a certain stoichiometric ratio. Its freezing point is significantly lower than the melting point of each pure component. It can be used for the treatment and modification of cellulose, effectively achieving efficient swelling and nano-dispersion of cellulose, promoting the self-delamination of cellulose, and generating quasi-cellulose filaments.

[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 (such as saliva) when a product containing a pH adjuster is dissolved or dispersed in it.

[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, 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.

[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 method for preparing nicotine pouch products, the specific steps of which are as follows:

[0075] Preparation of S1 and DES solutions includes the following steps:

[0076] (1) The hydrogen bond acceptor reagent and the hydrogen bond donor reagent are mixed in a molar ratio of 1:(1~4) to obtain the first mixed solution.

[0077] The hydrogen bond acceptor reagents include quaternary ammonium salts and / or zwitterions, such as choline chloride and betaine. The hydrogen bond donor reagents include one or more combinations of urea, thiourea, carboxylic acids, polyols, amino acids, sugars, and trifluoroacetamide; carboxylic acids include one or more combinations of phenylacetic acid, malic acid, citric acid, and succinic acid; polyols include one or more combinations of ethylene glycol, glycerol, butylene glycol, and xylitol; and sugars include glucose and / or fructose.

[0078] (2) Add 15-40% of the volume of the first mixed solution to the first mixed solution to obtain the second mixed solution, such that the concentration of the second mixed solution is 60-85% of the concentration of the first mixed solution.

[0079] (3) The second mixed solution is placed under a magnetic stirrer (purchased from Shanghai Meiyingpu Instrument Manufacturing Co., Ltd., MYP19-2 type magnetic stirrer) for heating and stirring. The heating temperature is 70~85℃ and the stirring time is 10~30 min. Stir until the solution is transparent to obtain the third mixed solution, which is the DES solution.

[0080] S2. Non-woven fabric pretreatment, including the following steps:

[0081] (1) The nonwoven fabric is immersed in the DES solution prepared in step S1 above. The immersion temperature is 50~70℃ and the immersion time is 2~5 h, so that a small amount of carboxyl groups are introduced on the nonwoven fabric to obtain the first nonwoven fabric.

[0082] (2) The first nonwoven fabric is washed with deionized water 2 to 5 times and then dried at 50 to 65°C for 1 to 3 hours to obtain the second nonwoven fabric, which is a nonwoven fabric containing carboxyl groups.

[0083] S3, Nicotine adsorption, includes the following steps:

[0084] (1) The carboxyl-containing nonwoven fabric prepared in step S2 (2) above is adsorbed in a nicotine source solution with a concentration of 50~150 mg / mL. The adsorption temperature is 24~30℃ and the adsorption time is 1~3 h to obtain the third nonwoven fabric.

[0085] The nicotine source includes one or more combinations of free nicotine, nicotine salts, nicotine-ion exchange resins, nicotine complexes, and non-covalently bound nicotine.

[0086] The 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.

[0087] (2) The third nonwoven fabric is washed with deionized water 2 to 5 times, and then dried at 50 to 65°C for 1 to 3 hours to obtain the fourth nonwoven fabric, which is a nonwoven fabric containing nicotine source.

[0088] S4. Preparation of nicotine pouch products includes the following steps:

[0089] (1) Mix 1.0~3.0 mg of nicotine source with a pH adjuster of 1.0~5.0% by weight of nicotine source to obtain a granular mixture, which is the nicotine-containing contents.

[0090] The pH adjuster is selected from acetic acid, adipic acid, citric acid, fumaric acid, gluconic acid-δ-lactone, gluconic acid, lactic acid, malic 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, potassium polyphosphate, carbonic acid, sodium carbonate, sodium bicarbonate, potassium carbonate, calcium carbonate, magnesium carbonate, magnesium oxide, metal hydroxides, or any combination thereof.

[0091] (2) The non-woven fabric containing nicotine source prepared in step (2) of S3 above is used as the outer packaging. The nicotine-containing contents are placed in the outer packaging. After cutting, hot pressing and ultraviolet sterilization, a nicotine bag product with a size of (1.2~2.5) cm×(1.5~3.0) cm and a weight of 1.0~3.0 g is obtained.

[0092] Example 1

[0093] (1) Mix choline chloride and citric acid in a molar ratio of 1:3 to obtain the first mixed solution;

[0094] (2) Add 20% of the volume of deionized water to the first mixed solution so that the concentration of the second mixed solution is 80% of the concentration of the first mixed solution;

[0095] (3) The second mixed solution is heated and stirred under a magnetic stirrer at a temperature of 80°C for 25 min until the solution becomes transparent, thus obtaining the third mixed solution, which is the DES solution.

[0096] (4) The nonwoven fabric is immersed in the DES solution prepared in step (3) above. The immersion temperature is 60°C and the immersion time is 2 h to obtain the first nonwoven fabric.

[0097] (5) The first nonwoven fabric is washed three times with deionized water and then dried at 60°C for 2 hours to obtain the second nonwoven fabric, which is a nonwoven fabric containing carboxyl groups.

[0098] (6) The carboxyl-containing nonwoven fabric prepared in step (5) above is placed in a free nicotine solution with a concentration of 100 mg / mL for adsorption. The adsorption temperature is 25℃ and the adsorption time is 2 h to obtain the third nonwoven fabric.

[0099] (7) The third nonwoven fabric prepared in step (6) above is washed three times with deionized water and then dried at 60°C for 2 hours to obtain the fourth nonwoven fabric, which is a nonwoven fabric containing nicotine, and is used as outer packaging.

[0100] (8) Mix 1 mg of nicotine malate with malic acid at a weight percentage of 1.0% of nicotine malate to obtain a granular mixture, which is the nicotine-containing contents;

[0101] (9) The nicotine-containing contents prepared in step (8) are placed in the nicotine-containing nonwoven fabric in step (7), and after cutting, hot pressing and ultraviolet sterilization, a nicotine bag product with a size of 2.0 cm × 2.0 cm and a weight of 1.5 g is obtained.

[0102] Example 2

[0103] (1) Mix choline chloride and citric acid in a molar ratio of 1:3 to obtain the first mixed solution;

[0104] (2) Add 20% of the volume of deionized water to the first mixed solution so that the concentration of the second mixed solution is 80% of the concentration of the first mixed solution;

[0105] (3) The second mixed solution is heated and stirred under a magnetic stirrer at a temperature of 80°C for 25 min until the solution becomes transparent, thus obtaining the third mixed solution, which is the DES solution.

[0106] (4) The nonwoven fabric is immersed in the DES solution prepared in step (3) above. The immersion temperature is 60°C and the immersion time is 3 h to obtain the first nonwoven fabric.

[0107] (5) The first nonwoven fabric is washed three times with deionized water and then dried at 60°C for 2 hours to obtain the second nonwoven fabric, which is a nonwoven fabric containing carboxyl groups.

[0108] (6) The carboxyl-containing nonwoven fabric prepared in step (5) above is adsorbed in a free nicotine solution with a concentration of 100 mg / mL. The adsorption temperature is 25℃ and the adsorption time is 2 h to obtain the third nonwoven fabric.

[0109] (7) The third nonwoven fabric prepared in step (6) above is washed three times with deionized water and then dried at 60°C for 2 hours to obtain the fourth nonwoven fabric, which is a nonwoven fabric containing nicotine, and is used as outer packaging.

[0110] (8) Mix 1 mg of nicotine malate with malic acid at a weight percentage of 1.0% of nicotine malate to obtain a granular mixture, which is the nicotine-containing contents;

[0111] (9) The nicotine-containing contents prepared in step (8) are placed in the nicotine-containing nonwoven fabric in step (7), and after cutting, hot pressing and ultraviolet sterilization, a nicotine bag product with a size of 2.0 cm × 2.0 cm and a weight of 1.5 g is obtained.

[0112] Example 3

[0113] (1) Mix choline chloride and citric acid in a molar ratio of 1:3 to obtain the first mixed solution;

[0114] (2) Add 20% of the volume of deionized water to the first mixed solution so that the concentration of the second mixed solution is 80% of the concentration of the first mixed solution;

[0115] (3) The second mixed solution is heated and stirred under a magnetic stirrer at a temperature of 80°C for 25 min until the solution becomes transparent, thus obtaining the third mixed solution, which is the DES solution.

[0116] (4) The nonwoven fabric is immersed in the DES solution prepared in step (3) above. The immersion temperature is 60°C and the immersion time is 2 h to obtain the first nonwoven fabric.

[0117] (5) The first nonwoven fabric is washed three times with deionized water and then dried at 60°C for 2 hours to obtain the second nonwoven fabric, which is a nonwoven fabric containing carboxyl groups.

[0118] (6) The carboxyl-containing nonwoven fabric prepared in step (5) above is adsorbed in a free nicotine solution with a concentration of 100 mg / mL. The adsorption temperature is 25℃ and the adsorption time is 2 h to obtain the third nonwoven fabric.

[0119] (7) The third nonwoven fabric prepared in step (6) above is washed three times with deionized water and then dried at 60°C for 2 hours to obtain the fourth nonwoven fabric, which is a nonwoven fabric containing nicotine, and is used as outer packaging.

[0120] (8) Mix 1 mg of nicotine malate with malic acid at a weight percentage of 1.0% of nicotine malate to obtain a granular mixture, which is the nicotine-containing contents;

[0121] (9) Place the nicotine-containing contents prepared in step (8) into the nicotine-containing nonwoven fabric in step (7), set the nicotine-containing nonwoven fabric as a double layer, and after cutting, hot pressing and ultraviolet sterilization, obtain a nicotine bag product with a size of 2.0cm×2.0cm and a weight of 1.5g.

[0122] Example 4

[0123] (1) Mix choline chloride and citric acid in a molar ratio of 1:3 to obtain the first mixed solution;

[0124] (2) Add 20% of the volume of deionized water to the first mixed solution so that the concentration of the second mixed solution is 80% of the concentration of the first mixed solution;

[0125] (3) The second mixed solution is heated and stirred under a magnetic stirrer at a temperature of 80°C for 25 min until the solution becomes transparent, thus obtaining the third mixed solution, which is the DES solution.

[0126] (4) The nonwoven fabric is immersed in the DES solution prepared in step (3) above. The immersion temperature is 60°C and the immersion time is 2 h to obtain the first nonwoven fabric.

[0127] (5) The first nonwoven fabric is washed three times with deionized water and then dried at 60°C for 2 hours to obtain the second nonwoven fabric, which is a low-modified nonwoven fabric containing a small amount of carboxyl groups.

[0128] (6) The nonwoven fabric is immersed in the DES solution prepared in step (3) above. The immersion temperature is 60°C and the immersion time is 3 h to obtain the third nonwoven fabric.

[0129] (7) The third nonwoven fabric was washed three times with deionized water and then dried at 60°C for 2 hours to obtain the fourth nonwoven fabric, which is a highly modified nonwoven fabric containing a large amount of carboxyl groups.

[0130] (8) The nonwoven fabrics containing a small amount of carboxyl groups and the nonwoven fabrics containing a large amount of carboxyl groups prepared in steps (5) and (6) above are adsorbed in tobacco extract with a concentration of 100 mg / mL. The adsorption temperature is 25℃ and the adsorption time is 2 h, respectively to obtain the fifth nonwoven fabric (i.e. obtained through the third nonwoven fabric) and the sixth nonwoven fabric (i.e. obtained through the fourth nonwoven fabric).

[0131] (9) The fifth and sixth nonwoven fabrics prepared in step (6) above are washed three times with deionized water and then dried at 60°C for 2 hours to obtain the seventh nonwoven fabric (i.e. obtained through the fifth nonwoven fabric) and the eighth nonwoven fabric (i.e. obtained through the sixth nonwoven fabric). The seventh and eighth nonwoven fabrics are combined to form a nonwoven fabric containing nicotine, which is used as outer packaging.

[0132] (10) Mix 1 mg of nicotine malate with malic acid at a weight percentage of 1.0% of nicotine malate to obtain a granular mixture, which is the nicotine-containing contents;

[0133] (11) Place the nicotine-containing contents prepared in step (8) above into the nicotine-containing nonwoven fabric in step (7) above. Set the nicotine-containing nonwoven fabric as a double layer, with the end closer to the contents being a highly modified nonwoven fabric (eighth nonwoven fabric) and the end further away from the contents being a low-modified nonwoven fabric (seventh nonwoven fabric). After slitting, hot pressing and ultraviolet sterilization, a nicotine bag product with a size of 2.0 cm × 2.0 cm and a weight of 1.5 g is obtained.

[0134] Comparative Example

[0135] This comparative example uses commercially available ZYN nicotine bags, the difference being that this comparative example uses ordinary non-woven fabric as the outer packaging.

[0136] Test Example: Nicotine In Vitro Release Test

[0137] To further illustrate the advantages of this patent, an in vitro nicotine release experiment was conducted on the nicotine pouch products in Examples 1-4 and the nicotine pouches in the comparative example. 100 mL of simulated artificial saliva with a pH of 6.8 was placed in each beaker and maintained at 37.0 ± 0.1°C. Nicotine pouch products or nicotine pouches with the same nicotine content were placed in each beaker and stirred at 100 rpm. A precise sample of 2 mL was taken every minute until 10 minutes. After 10 minutes, a sample was taken every 10 minutes, and 2 mL of simulated artificial saliva was added after each sample (to simulate the cumulative nicotine release in the oral cavity, artificial saliva was added after each sample as saliva was continuously secreted in the mouth). The 2 mL solution was diluted to 10 mL with simulated artificial saliva, and the nicotine content was detected by HPLC to calculate the relative cumulative nicotine release. A release rate curve was plotted with nicotine release rate on the ordinate and time on the abscissa (tested according to the current standard GB / T18886-2019 for artificial saliva).

[0138] The nicotine release curve results are as follows Figure 1 As shown, the nicotine release efficiency (also known as release rate) of the nicotine pouch products prepared through the embodiments of this application is significantly greater than that of the comparative example. Furthermore, the nicotine pouch products prepared in Examples 1-4 show a highly significant difference in nicotine release efficiency compared to the comparative example in the first 10 minutes, reaching a release rate of 85% at 40 minutes, exhibiting a gradual release that meets the requirements for sustained release. This indicates that the modified nonwoven fabric adsorbs a certain amount of nicotine and releases it in simulated oral cavity release, achieving the goal of synergistic nicotine release from the modified nonwoven fabric and the internally filled nicotine salts. Simultaneously, it overcomes the drawback of a slow nicotine release rate in the early stages of pouch use.

[0139] Therefore, it can be concluded that the nicotine pouch product and its preparation method provided by this patent introduce a small amount of carboxyl groups on the surface of nonwoven fabric using a eutectic solvent, thereby significantly improving the adsorption performance of nonwoven fabric for nicotine. The nicotine source is mixed with pH adjusters and other additives to prepare the contents. Then, using traditional processes, the contents are placed in a modified nonwoven fabric material, and the nicotine pouch product is obtained through shearing, hot pressing, and ultraviolet sterilization. This results in a release efficiency of ≥45.0% in the oral cavity from 0 to 10 minutes and ≥85.0% from 0 to 40 minutes, achieving stable nicotine release and good nicotine delivery. This allows a certain amount of nicotine to be released even before saliva has fully soaked the nonwoven fabric during the initial use of oral nicotine pouch products, compensating for the shortcomings of unclear nicotine release and delivery in the early stages of use, reducing oral irritation, providing richer flavor characteristics, reducing production costs, and enhancing the consumer experience.

[0140] 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.

[0141] 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.

[0142] The specific implementations given in this specification are examples of useful implementations of this patent. It will be apparent to those skilled in the art that this patent can be implemented using many variations of the equipment, equipment components, and method steps disclosed in this specification.

[0143] 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.

[0144] Furthermore, the scope of this patent should not be limited to any of the exemplary embodiments described above, but only to the appended claims and their equivalents.

Claims

1. A nicotine bagged product, characterized in that, The nicotine pouch product includes the contents and the outer packaging. The contents include a nicotine source; The outer packaging is prepared by adsorbing the nicotine source onto a nonwoven fabric under the action of a eutectic solvent.

2. The nicotine pouch product according to claim 1, characterized in that, The nonwoven fabric is immersed in the eutectic solvent, thereby attaching carboxyl groups to the nonwoven fabric. The soaking temperature is 50~55℃, 55~65℃ or 65~70℃; The soaking time is 2-3 hours, 3-4 hours, or 4-5 hours.

3. The nicotine pouch product according to claim 2, characterized in that, The eutectic solvent includes a hydrogen bond acceptor and a hydrogen bond donor, wherein the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 1:(1~4); The hydrogen bond acceptor reagent includes a quaternary ammonium salt and / or a zwitterion; the quaternary ammonium salt includes choline chloride, and the zwitterion includes betaine; The hydrogen bond donors include one or more combinations of urea, thiourea, carboxylic acids, polyols, amino acids, sugars, and trifluoroacetamide.

4. The nicotine pouch product according to claim 1, characterized in that, The nicotine source includes one or more combinations of free nicotine, nicotine salts, nicotine-ion exchange resins, nicotine complexes, and non-covalently bound nicotine.

5. The nicotine pouch product according to claim 1, characterized in that, The concentration of the nicotine source is 50-80 mg / mL, 80-100 mg / mL, or 100-150 mg / mL; The nonwoven fabric has an adsorption temperature of 24~25℃, 25~27℃ or 27~30℃ in the nicotine source; The nonwoven fabric adsorbs nicotine from the nicotine source for 1.0~1.5 h, 1.5~2.0 h, or 2.0~3.0 h.

6. The nicotine pouch product according to claim 1, characterized in that, The contents also include a pH adjuster, and the nicotine source is mixed with the pH adjuster to form particulate contents.

7. The nicotine pouch product according to claim 1, characterized in that, The size of the nicotine bagged product is (1.2~2.5)×(1.5~3.0) cm; The weight of the nicotine bagged product is 0.3~0.4 g, 0.4~0.6 g, 0.6~0.8 g, or 0.8~0.9 g.

8. The nicotine pouch product according to claim 7, characterized in that, The nicotine pouch product has a release efficiency of ≥45.0% in the oral cavity from minute 0 to minute 10; The nicotine pouch product has a release efficiency of ≥85.0% in the oral cavity from minute 0 to minute 40.

9. A method for preparing a nicotine pouch product according to any one of claims 1 to 8, characterized in that, Includes the following steps: Step A: The nonwoven fabric is pretreated in a eutectic solvent to obtain a nonwoven fabric containing carboxyl groups; Step B: The nonwoven fabric containing carboxyl groups is placed in the nicotine source for adsorption to obtain a nonwoven fabric containing nicotine; Step C: Mix the nicotine source with the additive to obtain the contents, place the contents in the non-woven fabric containing nicotine, and obtain the nicotine bagged product after shearing, hot pressing and ultraviolet sterilization.

10. The method for preparing nicotine pouch products according to claim 9, characterized in that, In step A, the pretreatment conditions are heating and stirring, the heating and stirring temperature is 80~95℃, and the heating and stirring time is 10~40 min; In step B, the adsorption temperature is 24~30℃, and the adsorption time is 1.0~3.0 h; In step C, the amount of additive added is 2.0 to 8.0% of the weight ratio of the nicotine source, and the nonwoven fabric containing nicotine is a single-layer nonwoven fabric or a double-layer nonwoven fabric. Specifically, the double-layer nonwoven fabric has a smaller nicotine source adsorption capacity at the end closer to the contents than at the end farther from the contents.

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