A mouth-held nicotine product and a method of making the same

Abstract

The application discloses a kind of oral nicotine products and preparation method thereof, belong to the field of smokeless tobacco products.The oral nicotine product is soft candy form, including nicotine component, coagulant, sweetener and alkaline pH regulator.The product can be homogeneous structure or double-layer structure, the nicotine content and / or pH regulator content of inner layer and outer layer in double-layer structure are different, so as to realize fast, moderate or slow differentiated release rate.The product of the application can relieve oral mucosa irritation, there is no solid waste, flexible in use, and can meet the individual needs of consumers for nicotine release rate.

Description

Technical Field

[0001] This invention relates to the field of tobacco products, specifically to a smokeless tobacco product, and more particularly to a nicotine-containing oral product and its preparation method. Background Technology

[0002] Smokeless tobacco products refer to tobacco products containing nicotine that are used orally, nasally, or topically without producing smoke. These include nicotine pouches (sheets, patches), tobacco products, chewing tobacco, tart tobacco, dissolved tobacco, and sniffing tobacco. According to Announcement No. 1 of 2026 issued by the State Tobacco Monopoly Administration, smokeless tobacco products are managed as cigarettes or tobacco products, strictly adhering to national restricted industry policies, and their production and sale are strictly prohibited without a license. This announcement further regulates the market order of smokeless tobacco products and also sets higher compliance requirements for the technological innovation of related products.

[0003] In recent years, smokeless tobacco products have developed rapidly worldwide, especially in the oral application sector. Due to the avoidance of harmful smoke produced by combustion and their discreet and convenient use, they have attracted increasing attention from consumers. Currently, the main types of smokeless oral tobacco products on the market are nicotine pouches and oral dissolving films. However, existing products still have significant shortcomings: First, nicotine pouches are placed between the lips and gums during use, and prolonged contact can cause continuous irritation to the oral mucosa, leading to burning sensations, discomfort, and even mucosal damage. Furthermore, the discarded pouches are solid waste, posing hygiene and safety hazards and negatively impacting environmental protection.

[0004] Secondly, while oral dissolving films are convenient to use, their rapid dissolution in the mouth and unadjustable nicotine release often result in the product being consumed before consumers have fully experienced physiological satisfaction, leading to a poor user experience. Furthermore, the limited nicotine content in oral dissolving films makes it difficult to meet the personalized needs of different consumers regarding release rate and intake.

[0005] Third, existing nicotine pouch products have been subject to strong technological barriers created by multinational tobacco companies (such as Philip Morris International) through extensive patent portfolios, posing numerous intellectual property obstacles for domestic companies to innovate in product structure, formulation, and usage methods.

[0006] Therefore, developing a new type of oral product that can alleviate oral mucosal irritation, autonomously regulate nicotine release rate, produce no solid waste after use, and comply with national regulations on smokeless tobacco products has significant market value and social importance. Summary of the Invention

[0007] To solve the above-mentioned technical problems, this patent provides the following technical solution: In a first aspect, a nicotine-containing product is provided, which is in the form of a soft candy and contains nicotine, a gelling agent, a sweetener, and an alkaline pH adjuster.

[0008] Furthermore, oral nicotine products have a double-layer structure, consisting of an inner layer and an outer layer, with different nicotine contents and / or pH adjuster contents in the inner and outer layers.

[0009] Furthermore, the outer layer has a higher nicotine content than the inner layer and / or the outer layer has a higher pH adjuster content than the inner layer. Alternatively, the outer layer has a lower nicotine content than the inner layer and / or the outer layer has a lower pH adjuster content than the inner layer.

[0010] Furthermore, the alkaline pH adjuster is selected from one or more of the following: calcium hydroxide, potassium hydroxide, sodium hydroxide, magnesium hydroxide, magnesium oxide, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, trisodium bicarbonate, calcium carbonate, sodium citrate, potassium citrate, monosodium citrate, disodium hydrogen phosphate, tripotassium phosphate, trisodium phosphate, sodium pyrophosphate, calcium lactate, sodium acetate, sodium gluconate, sodium L-malate, sodium DL-malate, potassium tartrate, arginine, and lysine.

[0011] Furthermore, the nicotine component is a nicotine salt selected from the following group: nicotine resinate, nicotine hydrochloride, nicotine phosphate, nicotine sulfate, nicotine pyruvate, nicotine formate, nicotine oxalate, nicotine ascorbate, nicotine glycolate, nicotine acetate, nicotine isovalerate, nicotine valerate, nicotine propionate, nicotine caprylate, nicotine lactate, nicotine acetylpropionate, nicotine sorbate, nicotine malate, nicotine fumarate, nicotine salicylate, nicotine glycinate, nicotine tartrate, nicotine succinate, and nicotine citric acid. Nicotine salts, nicotine benzoate, nicotine oleate, nicotine aconitate, nicotine butyrate, nicotine cinnamate, nicotine caprate, nicotine 3,7-dimethyl-6-octenate, nicotine 1-glutamate, nicotine heptamate, nicotine hexanoate, nicotine 3-hexenoate, nicotine trans-2-hexenoate, nicotine isobutyrate, nicotine laurate, nicotine 2-methylbutyrate, nicotine 2-methylvalerate, nicotine myristate, nicotine nonanoate, nicotine palmitate, nicotine 4-pentenoate, nicotine phenylacetate, nicotine 3-phenylpropionate.

[0012] Furthermore, the coagulant is selected from one or more of the following: gelatin, fish glue, gelatin, pectin, konjac gum, gum arabic, tragacanth gum, guar gum, locust bean gum, tamarind gum, tara gum, flaxseed gum, guar gum, fenugreek gum, soapberry gum, Indian gum, peach gum, sand wormwood gum, xanthan gum, gellan gum, guar gum, styrax polysaccharide, veslaw gum, casein, sodium caseinate, chitin, chitosan, whey protein isolate, whey protein concentrate, K-type carrageenan, I-type carrageenan, λ-type carrageenan, agar, sodium alginate, propylene glycol alginate, red algae gum, brown algae fucoidan, yeast polysaccharide, pullulan, sodium carboxymethyl cellulose, hydroxyethyl cellulose, microcrystalline cellulose, methyl cellulose, hydroxypropyl methyl cellulose, hydroxypropyl cellulose, modified starch, β-cyclodextrin, agar, agar-agar, and hygroscopic agar.

[0013] Furthermore, oral nicotine products may also contain one or more excipients selected from fruit juice, colorings, flavorings, and preservatives.

[0014] In a second aspect, a method for preparing an oral nicotine product of the first aspect is provided, comprising the following steps: S1. Mix the coagulant with a liquid medium (preferably water or fruit juice) and allow it to expand to obtain a mixture; S2. Heat the sweetener and water until completely dissolved and simmer until just boiling to obtain a syrup; S3. Add the mixture, nicotine component, pH adjuster and one or more excipients to the syrup, mix well to obtain a mixture; S4. Pour the mixture into a mold, cool and solidify to obtain a soft candy-like oral nicotine product.

[0015] Furthermore, in step S3, a layered casting or co-extrusion method is used to form a double-layered soft candy structure with inner and outer layers having different nicotine contents and / or pH adjuster contents.

[0016] This invention uses a soft candy form, which is soft in texture and smooth in surface. Compared with the fibrous material of nicotine pouches, it significantly reduces the physical irritation to the oral mucosa. Users can control the contact time and intensity between the product and the mucosa by chewing or sucking, further reducing discomfort.

[0017] By designing a dual-layer structure with different nicotine and / or pH adjuster contents in the inner and outer layers, three types of products can be prepared: fast-acting (high nicotine and high pH in the outer layer), slow-acting (low nicotine and low pH in the outer layer), and uniformly released. This allows consumers to personalize their needs for different onset speeds and levels of satisfaction. Furthermore, users can choose between chewing for accelerated release or sucking for slow release, allowing for self-adjustment. Attached Figure Description

[0018] 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.

[0019] Figure 1 Three different embodiments of the oral nicotine product according to the present invention are shown, wherein A represents a homogeneous oral nicotine product; B represents an oral nicotine product in which the nicotine content of the outer layer is higher than that of the inner layer and / or the pH adjuster content of the outer layer is higher than that of the inner layer; and C represents an oral nicotine product in which the nicotine content of the outer layer is lower than that of the inner layer and / or the pH adjuster content of the outer layer is lower than that of the inner layer. Figure 2 The nicotine release curves of Examples 1-3 as determined are shown. Detailed Implementation

[0020] 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.

[0021] In this specification and claims, several terms will be used, and unless otherwise indicated, these terms will be defined to have the following meanings: 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.

[0022] 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.

[0023] 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.

[0024] 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.

[0025] Unless otherwise specified, all embodiments and preferred embodiments mentioned herein can be combined to form new technical solutions.

[0026] Unless otherwise specified, all the technical features and preferred features mentioned herein can be combined to form new technical solutions.

[0027] 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.

[0028] 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.

[0029] 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.

[0030] 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).

[0031] Unless otherwise specified, percentages (%) in this document refer to percentages by mass relative to the composition.

[0032] Unless otherwise stated herein, the sum of the contents of the components in the composition is 100%.

[0033] 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.

[0034] Unless otherwise specified, the term "a" as used in this specification means "at least one".

[0035] 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.

[0036] 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.

[0037] 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.

[0038] One object of the present invention is to provide a nicotine-containing product in the form of a soft candy, comprising nicotine, a gelling agent, a sweetener, and an alkaline pH adjuster.

[0039] As used in this article, oral nicotine products are a type of smokeless tobacco product used in the oral cavity that does not produce smoke. Containing nicotine, they are absorbed into the body through the oral mucosa via methods such as holding or chewing, without involving combustion or inhalation. When used, oral nicotine products are placed on the oral mucosa (buccal or labial side). The nicotine is released slowly through saliva and oral temperature, absorbed into the bloodstream, and produces a feeling of physiological satisfaction. Compared to oral films or nicotine pouches, soft candy-like products support various usage methods such as holding, chewing, and sucking, allowing for adjustable release rates. Users can choose to slowly dissolve the nicotine to prolong the release duration or chew it more quickly to promote rapid nicotine release.

[0040] The "soft candy form" described in this invention refers to a product that has a gel-like texture, can be chewed or dissolved in the mouth, has a water content of 8%-20%, and can maintain its shape at room temperature but can be deformed by applying slight pressure.

[0041] As used herein, "nicotine ingredient" means any suitable form of nicotine intended to provide at least a portion of the oral absorption of nicotine, including, for example, nicotine and nicotine derivatives. Nicotine derivatives include one or more of nicotine salts, nicotine-ion exchange resins, nicotine complexes, and non-covalently bound nicotine.

[0042] As used in this article, "nicotine," also known as nicotine alkaloid, is an organic compound with the chemical formula C. 10 H 14 N2, with the structural formula shown in Formula I. Nicotine belongs to the alkaloid class of compounds. Alkaloids are a class of nitrogen-containing basic organic molecules that exhibit base-like chemical properties, forming salt solutes in water or reacting with acids. The nicotine structure contains a pyridine ring and a pyrrolidine ring, and its nitrogen atom readily accepts protons (H). + It is alkaline and can react with acids to form salt compounds.

[0043] (I)

[0044] In some embodiments, the nicotine component is a nicotine salt selected from the group consisting of: nicotine resinate, nicotine hydrochloride, nicotine phosphate, nicotine sulfate, nicotine pyruvate, nicotine formate, nicotine oxalate, nicotine ascorbate, nicotine glycolate, nicotine acetate, nicotine isovalerate, nicotine valerate, nicotine propionate, nicotine caprylate, nicotine lactate, nicotine acetylpropionate, nicotine sorbate, nicotine malate, nicotine fumarate, nicotine salicylate, nicotine glycinate, nicotine tartrate, nicotine succinate, nicotine citrate, etc. Citric acid salt, nicotine benzoate, nicotine oleate, nicotine aconitate, nicotine butyrate, nicotine cinnamate, nicotine caprate, nicotine 3,7-dimethyl-6-octenate, nicotine 1-glutamate, nicotine heptamate, nicotine hexanoate, nicotine 3-hexenoate, nicotine trans-2-hexenoate, nicotine isobutyrate, nicotine laurate, nicotine 2-methylbutyrate, nicotine 2-methylvalerate, nicotine myristate, nicotine nonanoate, nicotine palmitate, nicotine 4-pentenoate, nicotine phenylacetate, nicotine 3-phenylpropionate.

[0045] In some embodiments, the oral nicotine product has a two-layer structure, comprising an inner layer and an outer layer, wherein the nicotine content and / or pH adjuster content differs between the inner and outer layers. This includes three scenarios: the inner and outer layers have different nicotine contents but the same pH adjuster content; the inner and outer layers have the same nicotine content but different pH adjuster contents.

[0046] Nicotine is a weakly alkaline alkaloid that exists in aqueous solution in two interconvertible forms: free nicotine (unprotonated form, also known as nicotine salt) and protonated nicotine (nicotine salt form). The equilibrium between these two forms is entirely determined by the pH of the system. At lower pH values, nicotine is protonated (positively charged), existing as nicotine salt. When the pH rises to an alkaline range, nicotine loses protons, converting into uncharged free nicotine. Free nicotine is electrically neutral and highly lipid-soluble, thus penetrating the phospholipid bilayer of oral mucosal cells more efficiently. Conversely, protonated (salt form) nicotine, due to its high charge and water solubility, has extremely low transmembrane capacity. Therefore, adding alkaline pH adjusters can promote the release of free nicotine from nicotine salt in the oral environment, allowing for efficient absorption through the oral mucosa and achieving physiological satisfaction.

[0047] In a bilayer structure, even if the nicotine content is the same in the inner and outer layers, different pH adjuster contents will result in different nicotine release and absorption effects.

[0048] In some implementations, the nicotine content of the outer layer is higher than that of the inner layer. Alternatively, the pH adjuster content of the outer layer is higher than that of the inner layer. Or, the nicotine content of the outer layer is higher than that of the inner layer, and the pH adjuster content of the outer layer is also higher than that of the inner layer.

[0049] In other embodiments, the nicotine content of the outer layer is lower than that of the inner layer. Alternatively, the pH adjuster content of the outer layer is lower than that of the inner layer. Or, the nicotine content of the outer layer is lower than that of the inner layer, and the pH adjuster content of the outer layer is higher than that of the inner layer.

[0050] In some embodiments, the alkaline pH adjuster is selected from one or more of the following: calcium hydroxide, potassium hydroxide, sodium hydroxide, magnesium hydroxide, magnesium oxide, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, trisodium bicarbonate, calcium carbonate, sodium citrate, potassium citrate, monosodium citrate, disodium hydrogen phosphate, tripotassium phosphate, trisodium phosphate, sodium pyrophosphate, calcium lactate, sodium acetate, sodium gluconate, sodium L-malate, sodium DL-malate, potassium tartrate, arginine, and lysine.

[0051] In some embodiments, the coagulant is selected from one or more of the following: gelatin, fish glue, gelatin, pectin, konjac gum, gum arabic, tragacanth gum, guar gum, locust bean gum, tamarind gum, tara gum, flaxseed gum, guar gum, fenugreek gum, soapberry gum, Indian gum, peach gum, sand wormwood gum, xanthan gum, gellan gum, guar gum, styrax polysaccharide, veslaw gum, casein, sodium caseinate, chitin, chitosan, whey protein isolate, whey protein concentrate, K-type carrageenan, I-type carrageenan, λ-type carrageenan, agar, sodium alginate, propylene glycol alginate, red algae gum, brown algae fucoidan, yeast polysaccharide, pullulan, sodium carboxymethyl cellulose, hydroxyethyl cellulose, microcrystalline cellulose, methyl cellulose, hydroxypropyl methyl cellulose, hydroxypropyl cellulose, modified starch, β-cyclodextrin, agar, agar-agar, and hygroscopic agar.

[0052] The coagulants used in this article must be absorbable by humans. Non-limiting examples of suitable coagulants include xanthan gum, carrageenan and its derivatives, glucan gum, hydroxypropyl methylcellulose, fungal gums and their derivatives, pullulan, rhamnose gum, Brunei gum, konjac, gelling polysaccharides, carbomer, alginate, alginic acid, alginate and its derivatives, hydroxyethyl cellulose and its derivatives, hydroxypropyl cellulose and its derivatives, starch phosphate derivatives, guar gum and its derivatives, starch and its derivatives, copolymers of maleic anhydride and olefins and their derivatives, ethylene glycol / propylene glycol copolymers, long-chain alcohols such as docosyl alcohol, poloxamer and its derivatives, polyacrylates and their derivatives, methylcellulose and its derivatives, ethylcellulose and its derivatives. Agar and its derivatives, gum arabic and its derivatives, pectin and its derivatives, chitosan and its derivatives, high molecular weight polyethylene glycols such as polyethylene glycol (molecular weight of 10,000 and above), ebony gum, carob gum, natto gum, copolymers of ethylene pyrrolidone and olefins, tragacanth gum, polyacrylamide, chitin derivatives, gelatin, β-glucan, dextrin, dextran, cyclodextrin, methacrylates, microcrystalline cellulose, polyquaternium salts, D-galactose gum, Indian gum, psyllium gum, tung oil, tamarind gum, larch gum, talc, kaolin clay, bentonite, cellulose, pyrolytic silica, and mixtures thereof. The preferred ingredients are xanthan gum, carrageenan and its derivatives, glycan gum, hydroxypropyl methylcellulose, fungal gums and their derivatives, pullulan, rhamnose gum, Brunei gum, konjac, gelatin, carbomer, alginate, alginic acid, alginate and its derivatives, hydroxyethyl cellulose and its derivatives, hydroxypropyl cellulose and its derivatives, starch phosphate derivatives, guar gum and its derivatives, starch and its derivatives, copolymers and derivatives of maleic anhydride and olefins, cellulose gum and its derivatives, poloxamer and its derivatives, gelatin, and mixtures thereof.

[0053] The soft candy-like nicotine product described in this invention can be processed into various geometric and biomimetic shapes to suit different consumption scenarios and aesthetic needs, such as: spheres, ellipsoids, oblate spheroids, cylinders, frustums, cubes, cuboids, tetrahedrons, octahedrons, rings, semicircles, triangles, hearts, stars, crescents, flowers, animal shapes, fruit shapes, letter shapes, number shapes, and the semi-elliptical shape with a concave bottom unique to QQ candies. These shapes can be achieved through mold casting or extrusion cutting, and the different shapes have slightly different tactile sensations and release rates when dissolved or chewed in the mouth, enriching the consumer's user experience.

[0054] In some embodiments, oral nicotine products also contain one or more excipients selected from fruit juice, colorings, flavorings, and preservatives.

[0055] Non-limiting examples of flavorings include peppermint, cinnamon, cherry, coconut, coffee, chocolate, vanilla, citrus (such as grapefruit, orange, lime, bergamot, or lemon), menthol, licorice, caramel, honey, peanut, walnut, cashew, hazelnut, almond, pineapple, strawberry, raspberry, tropical fruit, cherry, cinnamon, peppermint, deer hoof grass, spearmint, eucalyptus, apple, pear, peach, strawberry, apricot, raspberry, cherry, pineapple, lemongrass, lime, chili, capsaicin, citrus, tobacco flavor, bergamot, smoky flavoring, plum, eucalyptus, clove, bay leaf, fennel, thyme, cedar leaf, and nutmeg flavorings.

[0056] The soft candy-like oral nicotine product of this invention can use a variety of natural fruit juices, concentrated fruit juices, or fruit pulps as flavoring agents. According to the fruit source, it can be divided into citrus fruits (such as sweet orange juice, lemon juice, lime juice, tangerine juice, grapefruit juice, kumquat juice), pome fruits (such as apple juice, pear juice, hawthorn juice), stone fruits (such as peach juice, apricot juice, cherry juice, plum juice), berries (such as strawberry juice, blueberry juice, raspberry juice, blackberry juice, cranberry juice, mulberry juice, raspberry juice, blackcurrant juice, kiwi juice, pomegranate juice), tropical fruits (such as mango juice, pineapple juice, passion fruit juice, gravy juice, coconut juice, banana juice, papaya juice, dragon fruit juice, guava juice, star fruit juice, mangosteen juice, prickly pear juice, custard apple juice, cantaloupe juice, watermelon juice), as well as unique and other types of fruit juices such as grape juice, fig juice, sea buckthorn juice, goji berry juice, and also include special flavored fruit juices such as elderberry juice and acerola cherry juice. According to the processing form, it can be classified as freshly squeezed juice (NFC non-concentrated juice), concentrated juice (FC), fruit pulp, fruit puree, concentrated fruit pulp, clear juice (such as apple juice), cloudy juice (such as orange juice), juice powder or solid fruit juice beverage, etc.

[0057] The soft candy-like nicotine product of this invention can be formulated with various colorants to give the product an appealing color. From a natural source perspective, there is a rich variety of natural pigments that can be extracted from plants. Red pigments include beetroot red, extracted from beetroot and commonly used for coloring candies and baked goods; capsicum red, extracted from chili peppers, ranging from orange-red to red; and red yeast rice red, produced by fermenting rice with Monascus purpureus, ranging from red to purplish-red. Yellow pigments include turmeric, extracted from turmeric rhizomes, bright yellow and widely used in candies and seasonings; gardenia yellow, extracted from gardenia fruit, ranging from yellow to orange-yellow; safflower yellow, extracted from safflower, bright yellow; citrus yellow, extracted from citrus peel, orange-yellow; and lutein, derived from plants such as marigolds. Extracted from various sources, it ranges in color from yellow to orange-yellow; blue pigments include gardenia blue, made from components of gardenia fruit through enzymatic treatment, and phycocyanin, extracted from spirulina and other cyanobacteria, which is a bright blue; green pigments include sodium copper chlorophyll, extracted from plant leaves and copper-treated, which is a bright green and has good stability in solid foods; purple pigments include lithospermum erythrorhizon, extracted from the root of lithospermum erythrorhizon, which ranges in color from purple to red, and shellac, extracted from the resin secreted by lac insects, which is purplish-red; black pigments include plant carbon black, made from plant materials through carbonization, which is black and commonly used for black coloring candies, and cocoa shell coloring, extracted from cocoa bean shells, which ranges in color from brown to dark brown. From animal sources, cochineal red is a natural pigment extracted from female cochineal insects, which is deep red and commonly used for red coloring candies, jellies, and beverages. From mineral sources, titanium dioxide, also known as titanium white, is white and gives products a white, opaque appearance, often used in candy coatings. Natural pigments used in appropriate amounts according to production needs include citrus yellow, sorghum red, and beet red. Sorghum red, extracted from sorghum husks, is reddish-brown and can be used in various foods as needed. Caramel color, made from sugars through a caramelization reaction, is brown to dark brown and is one of the most commonly used brown coloring agents in candy. Regarding synthetic pigments, those permitted for use in candy in my country mainly include lemon yellow (yellow), sunset yellow (orange-yellow), carmine (red), amaranth (reddish-purple), brilliant blue (bright blue), indigo (deep blue), erythrosine (red, bright color), allura red (red, strong coloring power), and new red (red). These synthetic pigments are characterized by bright color, strong coloring power, good stability, and low cost. When used in candy within prescribed limits, they can achieve a bright and long-lasting color effect. For candy products with a coating layer, quinoline yellow and its aluminum lake, which are yellow, are also permitted, but only for candy coatings. Regarding inorganic pigments, iron oxide red and iron oxide black, appearing as red and black respectively, are used in extremely small amounts and can be used for fine-tuning the color of candies. Combinations of one or more of the above colorants can give soft candies a rich variety of color appearances, enhancing the product's visual appeal.

[0058] Preservatives may include at least one of ethylparaben, benzoic acid, benzoate, sorbic acid, sorbate, calcium propionate, sodium diacetate, sodium lactate, propylparaben, and sodium dehydroacetate.

[0059] Another object of the present invention is to provide a method for preparing oral nicotine products, comprising the following steps: S1. Mix the coagulant with the fruit juice and let it soak to obtain a mixture; S2. Heat the sweetener and water until completely dissolved and simmer until just boiling to obtain a syrup; S3. Add the mixture, nicotine component, pH adjuster and one or more excipients to the syrup, mix well to obtain a mixture; S4. Pour the mixture into a mold, cool and solidify to obtain a soft candy-like oral nicotine product.

[0060] In some embodiments, the process also includes step S5, a drying step. For example, the oral nicotine product is placed on a stainless steel mesh rack and dried in a constant temperature drying oven at 30°C and 50% relative humidity for 8 hours to allow surface moisture to evaporate.

[0061] In some implementations, the pH is adjusted to 7.5-9.0 in step S3.

[0062] In some embodiments, step S3 employs a layered casting or co-extrusion method to form a bilayer soft candy structure with inner and outer layers having different nicotine and / or pH adjuster contents.

[0063] Layered casting is the most direct technique for preparing multi-layered candies. Its basic principle is to inject liquids of different compositions into the same mold in stages, achieving interlayer bonding by controlling the solidification timing of each layer. The specific steps are as follows: First, prepare the inner and outer layer liquids. First, pour the outer layer liquid into the mold, placing the mold in a cooling environment to allow the surface of the outer layer liquid to partially or completely solidify, forming an outer shell with a certain strength. Then, pour the inner layer liquid into the solidified outer cavity until the mold is full. Finally, allow the entire mold to cool completely, allowing the inner layer to solidify completely, resulting in a double-layered soft candy with an outer layer enclosing the inner layer.

[0064] Co-extrusion is a method that uses a coaxial extruder or multi-channel extrusion equipment to simultaneously extrude two or more liquid materials with different compositions to form a concentric layered structure. The specific steps are as follows: Inner layer and outer layer liquid materials are prepared separately and placed in two independent hoppers, then pumped to the co-extrusion die by a metering pump. The co-extrusion die typically has an annular or coaxial structure. The outer layer liquid flows out from the outer annular channel, and the inner layer liquid flows out from the central channel. The two materials converge at the die exit and are extruded together to form a continuous strip with outer and inner layers. This strip is rapidly solidified through a cooling tunnel or cooling water tank, and then cut to a predetermined length by a cutting device to obtain a multi-layered soft candy.

[0065] In some embodiments, the coagulant is selected from one or more of gelatin, fish glue, gelatin, carrageenan, agar, pectin, konjac gum, xanthan gum, gellan gum, guarana gum, sodium alginate, sodium carboxymethyl cellulose, or modified starch.

[0066] In some embodiments, the amount of the coagulant used is 1% to 30% of the total mass of the oral nicotine product. In some embodiments, the amount of the coagulant used is 5% to 20% of the total mass.

[0067] In some embodiments, the soaking is carried out at room temperature for 10 to 60 minutes. In some embodiments, the soaking is carried out at a low temperature of 4 to 25 degrees Celsius for 30 to 120 minutes.

[0068] In some embodiments, the mass ratio of the coagulant to the fruit juice is 1:2 to 1:10. In some embodiments, the mass ratio is 1:3 to 1:6. In some embodiments, the soaking process is accompanied by low-speed stirring at 20 to 100 rpm to promote the coagulant's full absorption of the fruit juice and the formation of a uniform paste-like mixture.

[0069] In some embodiments, the sweetener is selected from one or more of sucrose, white sugar, glucose, fructose, maltose, high-fructose corn syrup, corn syrup, maltose syrup, sorbitol, xylitol, erythritol, maltitol, steviol glycosides, mogrosides, aspartame, acesulfame potassium, sucralose, or cyclamate.

[0070] In some embodiments, the sweetener is used in an amount of 30% to 80% of the total mass of the oral nicotine product. In some embodiments, the sweetener is used in an amount of 50% to 70% of the total mass.

[0071] In some embodiments, the heating and cooking are carried out under normal pressure at a temperature of 100°C to 130°C. Alternatively, the heating temperature may be 110°C to 120°C. During the cooking process, continuous stirring is maintained at a speed of 30 to 150 revolutions per minute to prevent localized caramelization of the syrup.

[0072] In some embodiments, the mixture, nicotine components, and pH adjuster are added after the syrup has been cooled to 80 to 110 degrees Celsius to avoid the high temperature destroying the nicotine.

[0073] In some embodiments, the mold is made of food-grade silicone, polycarbonate, or stainless steel. In some embodiments, the inner cavity shape of the mold is selected from spherical, ellipsoidal, cylindrical, cubic, heart-shaped, star-shaped, animal-shaped, or fruit-shaped.

[0074] Example

[0075] Table 1. Names of Raw Materials and Suppliers

[0076] Table 2. Instruments used in the experiment and their suppliers

[0077] Example 1

[0078] Table 3. Raw material ratio

[0079] Total nicotine content (based on pure nicotine): 0.40g (approximately 4mg / capsule, approximately 100 capsules total, approximately 1g per capsule)

[0080] 2. Preparation process

[0081] S1 Soaking: Sprinkle 20.0g of gelatin powder into 30.0g of apple juice, stir gently with a glass rod to completely wet the powder, and let stand at room temperature (25℃) for 30 minutes until the gelatin powder fully absorbs water and expands to form a translucent gel mixture.

[0082] S2 Sugar Cooking: Add 45.0g of granulated sugar, 50.0g of maltose syrup, and 15.0g of purified water to a stainless steel pot. Place the pot on an induction cooker and heat over low heat (approximately 300W), stirring continuously with a silicone spatula. When the sugar is completely melted, the solution becomes transparent, and begins to boil slightly (temperature approximately 115℃), immediately stop heating.

[0083] S3 Cooling and Mixing: Transfer the cooked syrup to a water bath and cool to 90°C. Add the soaked gelatin-juice mixture and homogenize at 5000 rpm for 2 minutes until homogeneous. Then add 1.67g of nicotine resinate, 0.40g of baking soda, and 0.10g of sodium citrate, and continue homogenizing at 8000 rpm for 3 minutes to ensure all solids are completely dissolved and dispersed. At this point, measure the pH of the mixture with a pH meter; the measured value is 8.6, which is within the target range of 7.5-9.0, requiring no further adjustment.

[0084] S4 Injection and Solidification: Maintain the mixture at 80°C and inject it into the pre-placed spherical silicone molds using a disposable dropper or injection gun (approximately 1.0 mL per cavity). After filling, gently shake the mold to remove air bubbles. Place the molds in the refrigerator (4°C) and allow them to solidify for 6 hours.

[0085] S5 Demolding and Drying: Remove the mold and carefully push the formed QQ candy out of the silicone mold. Place the QQ candy on a stainless steel mesh rack and dry it in a constant temperature drying oven at 30℃ and 50% relative humidity for 8 hours to allow surface moisture to evaporate. Approximately 100 yellow, transparent, smooth, and moderately elastic spherical nicotine QQ candies are obtained, each weighing approximately 1g and containing approximately 4mg of pure nicotine.

[0086] Example 2

[0087] Table 4. Outer Layer Formulation

[0088] Table 5. Inner Layer Formulation

[0089] Total nicotine content (based on pure nicotine): outer layer 0.08g + inner layer 0.32g = 0.40g.

[0090] 3. Preparation process (layered casting method)

[0091] S1 Prepare the material solutions independently according to the outer layer and inner layer formulations: The preparation steps of the outer layer material solution are the same as S1-S3 in Example 1, and the pH is adjusted to about 7.8; the pH of the inner layer material solution is adjusted to about 8.8.

[0092] S2. Pre-cool the spherical silicone mold in an ice-water bath for 10 minutes. First, pour the outer layer of liquid material into each mold cavity to 1 / 2 the height (about 0.5 mL), with the liquid temperature at 80℃ during pouring. Move the mold into a refrigerator (4℃) and let it stand for 15 minutes to allow the surface of the outer layer of liquid material to solidify and form a semi-solid shell.

[0093] S3 Remove the mold and carefully inject the inner layer liquid (80℃) into the solidified outer shell using an injection needle until the mold cavity is filled (approximately 1.0 mL). Be careful to avoid puncturing the bottom of the outer layer.

[0094] S4 Place the filled mold in a 4°C refrigerator and let it stand overnight to allow the inner layer to solidify completely.

[0095] S5 Demolding and drying: Same as step S5 in Example 1. Approximately 100 double-layered spherical QQ candies are obtained, with a light yellow outer layer and a dark yellow inner layer. The surface is smooth. When chewing, the low-nicotine outer layer is felt first, followed by the release of the high-nicotine inner layer after biting through, resulting in a delayed sense of satisfaction.

[0096] Example 3

[0097] Table 6. Outer Layer Formulation

[0098] Table 7. Inner Layer Formulation

[0099] Total nicotine content (based on pure nicotine): outer layer 0.32g + inner layer 0.08g = 0.40g.

[0100] 3. Preparation process

[0101] The same layered casting method as in Example 2 was used, but with the following difference: the outer layer was a high-nicotine, high-pH formula, while the inner layer was a low-nicotine, low-pH formula. The outer layer was first poured into the mold halfway up, and after it solidified, the inner layer was poured in. All other conditions remained exactly the same.

[0102] The final product has a similar appearance to Example 2, but the outer layer has a high concentration of nicotine. When consumers put it in their mouths, the outer layer quickly releases a high dose of free nicotine, producing a strong and rapid sense of satisfaction.

[0103] Test Example

[0104] 1. Nicotine release curve determination

[0105] The dissolution medium was phosphate buffer solution at pH 6.8 (simulating the neutral environment of the oral cavity), with a volume of 50 mL, a temperature of 37 °C, and a rotation speed of 50 rpm. Ten whole QQ candies (approximately 1 g each, containing approximately 4 mg of nicotine) prepared in Examples 1-3 were taken from each group and placed into dissolution vessels. 5 mL samples were taken at predetermined time points, and an isothermal and equal-volume blank medium was added simultaneously. After filtering through a 0.45 μm filter membrane, the nicotine concentration was determined by high-performance liquid chromatography (HPLC). Chromatographic conditions: C18 column (4.6 × 250 mm, 5 μm), mobile phase: methanol: 0.1% phosphoric acid aqueous solution (50:50), flow rate 1.0 mL / min, detection wavelength 260 nm, injection volume 20 μL. The results are shown below. Figure 2 .

[0106] 2. Sensory evaluation

[0107] Evaluation Methodology: Thirty healthy adult volunteers (aged 25-45, 15 men and 15 women) with experience using nicotine pouches were recruited using a double-blind, randomized, crossover design. Each volunteer used one pouch each of Examples 1, 2, and 3 (each containing 4mg of nicotine) on three different days, with intervals of at least 48 hours between each use. After using the product, volunteers were asked to rate the following dimensions (1-10 points) within 0-60 minutes: 1) Initial physiological satisfaction intensity (at 1 minute); 2) Time to reach maximum satisfaction (in minutes). Any discomfort was also recorded.

[0108] Table 8. Evaluation Results

[0109] Dissolution data show significant differences in nicotine release rates among the three examples: Example 3 (high nicotine and high pH in the outer layer) released the fastest; Example 1 (uniform type) had a moderate release rate; and Example 2 (low nicotine and low pH in the outer layer) released the slowest. Sensory evaluation results were highly consistent with the dissolution data. Example 3 provided volunteers with a strong sense of satisfaction within 1 minute, reaching maximum satisfaction in just 2.8 minutes; Example 1's indicators were moderate; and Example 2 had the slowest onset of action, with a delayed intensity of satisfaction.

[0110] 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.

[0111] 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.

[0112] 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.

[0113] 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-containing product, characterized in that, The oral nicotine product is in the form of a soft candy, and contains nicotine, a gelling agent, a sweetener, and an alkaline pH adjuster.

2. The oral nicotine product according to claim 1, characterized in that, The oral nicotine product has a double-layer structure, which includes an inner layer and an outer layer. The nicotine content of the inner layer and the outer layer are different and / or the pH adjuster content of the inner layer and the outer layer is different.

3. The oral nicotine product according to claim 2, characterized in that, The nicotine content of the outer layer is higher than that of the inner layer and / or the pH adjuster content of the outer layer is higher than that of the inner layer.

4. The oral nicotine product according to claim 2, characterized in that, The nicotine content of the outer layer is lower than that of the inner layer and / or the pH adjuster content of the outer layer is lower than that of the inner layer.

5. The oral nicotine product according to any one of claims 1-4, characterized in that, The alkaline pH adjuster is selected from one or more of the following: calcium hydroxide, potassium hydroxide, sodium hydroxide, magnesium hydroxide, magnesium oxide, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, trisodium bicarbonate, calcium carbonate, sodium citrate, potassium citrate, monosodium citrate, disodium hydrogen phosphate, tripotassium phosphate, trisodium phosphate, sodium pyrophosphate, calcium lactate, sodium acetate, sodium gluconate, sodium L-malate, sodium DL-malate, potassium tartrate, arginine, and lysine.

6. The oral nicotine product according to any one of claims 1-5, characterized in that, The nicotine component is a nicotine salt selected from the group consisting of: nicotine resinate, nicotine hydrochloride, nicotine phosphate, nicotine sulfate, nicotine pyruvate, nicotine formate, nicotine oxalate, nicotine ascorbate, nicotine glycolate, nicotine acetate, nicotine isovalerate, nicotine valerate, nicotine propionate, nicotine caprylate, nicotine lactate, nicotine acetylpropionate, nicotine sorbate, nicotine malate, nicotine fumarate, nicotine salicylate, nicotine glycinate, nicotine tartrate, nicotine succinate, and nicotine citrate. Nicotine benzoate, nicotine oleate, nicotine aconitate, nicotine butyrate, nicotine cinnamate, nicotine caprate, nicotine 3,7-dimethyl-6-octenate, nicotine 1-glutamate, nicotine heptamate, nicotine hexanoate, nicotine 3-hexenoate, nicotine trans-2-hexenoate, nicotine isobutyrate, nicotine laurate, nicotine 2-methylbutyrate, nicotine 2-methylvalerate, nicotine myristate, nicotine nonanoate, nicotine palmitate, nicotine 4-pentenoate, nicotine phenylacetate, nicotine 3-phenylpropionate.

7. The oral nicotine product according to any one of claims 1-6, characterized in that, The coagulant is selected from one or more of the following: gelatin, fish glue, gelatin, pectin, konjac gum, gum arabic, tragacanth gum, guar gum, locust bean gum, tamarind gum, tara gum, flaxseed gum, guar gum, fenugreek gum, soapberry gum, Indian gum, peach gum, sand wormwood gum, xanthan gum, gellan gum, guar gum, styrax polysaccharide, veslaw gum, casein, sodium caseinate, chitin, chitosan, whey protein isolate, whey protein concentrate, K-type carrageenan, I-type carrageenan, λ-type carrageenan, agar, sodium alginate, propylene glycol alginate, red algae gum, brown algae fucoidan, yeast polysaccharide, pullulan, sodium carboxymethyl cellulose, hydroxyethyl cellulose, microcrystalline cellulose, methyl cellulose, hydroxypropyl methyl cellulose, hydroxypropyl cellulose, modified starch, β-cyclodextrin, agar, agar-agar, and hygroscopic agar.

8. The oral nicotine product according to any one of claims 1-7, characterized in that, The oral nicotine products also contain one or more excipients selected from fruit juice, coloring, flavoring, and preservatives.

9. A method for preparing an oral nicotine product according to any one of claims 1-8, characterized in that, Includes the following steps: S1. Mix the coagulant with the liquid medium and allow it to expand to obtain a mixture; S2. Heat the sweetener and water until completely dissolved and simmer until just boiling to obtain a syrup; S3. Add the mixture, nicotine component, pH adjuster and one or more excipients to the syrup, mix well to obtain a mixture; S4. Inject the mixture into a mold, cool and solidify to obtain a soft candy-like oral nicotine product.

10. The method according to claim 9, characterized in that, In step S3, a layered casting or co-extrusion method is used to form a double-layered soft candy structure with inner and outer layers having different nicotine contents and / or pH adjuster contents.

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