Oral nicotine product containing free-state nicotine and nicotine salt, and preparation method therefor

Abstract

An oral nicotine product containing free-state nicotine and nicotine salt. The product contains the free-state nicotine, the nicotine salt, a matrix, Quercus variabilis, Chinese liquorice, water, and an additive. Further disclosed is an oral nicotine product, containing a guarana extract, a matrix, Quercus variabilis, Chinese liquorice, water, and an additive.

Description

An oral nicotine product containing free nicotine and nicotine salt and a preparation method thereof

[0001] Related applications

[0002] This application claims priority to Chinese patent application No. 202311221471.0, filed on September 20, 2023, entitled “An oral nicotine product containing free nicotine and nicotine salts,” the entire text of which is hereby incorporated by reference. Technical Field

[0003] The present application relates to the field of tobacco, and in particular to an oral nicotine product containing free nicotine and nicotine salts and a preparation method thereof. Background Art

[0004] Snus, a smokeless tobacco product, has been used in Europe for hundreds of years. Traditional snus is made by powdering dried tobacco leaves, sterilizing them, adding flavor, and humidifying them, then placing them in saliva-permeable pouches. The pouches are then placed between the lips and gums. After being soaked in saliva, the nicotine in the tobacco leaves seeps through the pouches, is absorbed through the mucous membranes, and quickly enters the bloodstream, achieving the desired physiological experience of smoking cigarettes. Compared to traditional cigarettes, where nicotine is released through combustion and absorbed through the lungs, snus is made from tobacco leaves. Nicotine in snus is absorbed through saliva, making it safer and more environmentally friendly. However, the rate and amount of nicotine released are limited. Furthermore, with long-term snus use, the pigments in the tobacco leaves can be deposited on the teeth and mucous membranes, making them difficult to clean.

[0005] With the advancement of free nicotine extraction and synthesis technologies, adding free nicotine to snus is becoming a reality. As a new form of nicotine ingestion in smokeless tobacco, this new smokeless tobacco product uses a white edible material as a filler, along with nicotine or nicotine salts, flavorings, and humectants. This not only improves the pigmentation problem of snus, but also, by adding nicotine externally, increases the nicotine release rate while meeting the varying nicotine content requirements of different demographics. Currently, commercially available nicotine snus uses primarily free nicotine, nicotine salts, and nicotine cation exchange resins. Because natural or synthetic flavorings are weakly acidic, the addition of an organic or inorganic base as a pH adjuster allows the nicotine to be rapidly absorbed by the mucous membranes in its free form when placed between the gums and lips.

[0006] Commercially available products include British American Tobacco's Velo brand snus, a free-nicotine snus product. The addition of free nicotine in this product provides consumers with a long-lasting sense of satisfaction during the mouthful. However, if the amount of free nicotine added to this product is too low, the product's release time is too short, making it difficult for users to achieve long-term satisfaction. However, if the nicotine content is increased, the throat hit of the free nicotine will be too strong, resulting in a low level of mouthfeel.

[0007] An existing patent (patent application number: 201280017683.0) discloses a pouch containing nicotine in the form of a free salt. The pouch contains free salt, a pH regulator, and a filler, wherein the filler is a combination of sugars, cellulose, flavoring agents, and other additives. This product uses nicotine salt to replace the free nicotine in traditional snus, with each pouch containing nicotine salts ranging from 0.5mg to 9mg. The nicotine salt in this product can be rapidly absorbed through the oral mucosa, and the product has a slightly lower irritation, significantly improving the user's taste experience. However, the nicotine salt can diffuse from the product into the human oral cavity within 5-8 seconds, resulting in a very short period of physiological satisfaction during the user's experience of the product.

[0008] For the above-mentioned patented products or commercially available products, whether they are single free nicotine or nicotine salt oral tobacco products, and regardless of the amount of free nicotine or nicotine salt added, there is a problem that it is difficult to meet the user's physiological experience requirements. In addition, among the raw materials of the above-mentioned products, the filler matrix generally uses microcrystalline cellulose. Although it is low-cost and easy to manufacture, the oral tobacco products made from it tend to form a paste-like hard mass when chewed, and the chewing comfort is low. In addition, in order to improve the taste and enhance the consumer's experience of use, a certain amount of sweetness, fragrance and other additives will be used in the product. However, since the total amount of material in a single bag is fixed, the release of the additives is the same as nicotine, and it is difficult to achieve a long-term and flat taste.

[0009] Summary of the Invention

[0010] Some embodiments of the present application provide an oral nicotine product containing free nicotine and nicotine salts.

[0011] In a first aspect, an oral nicotine product containing free nicotine and nicotine salts is provided, comprising free nicotine, nicotine salts, a matrix, cork oak, licorice, water, and additives.

[0012] In some embodiments, the product comprises, by mass percentage, about 0.3% to about 4% free nicotine, about 0.75% to about 10% nicotine salt, about 20% to about 50% matrix, about 3% to about 20% cork oak, about 2% to about 10% licorice, about 5% to about 30% water, and the remainder being additives.

[0013] In some embodiments, the pH of the preparation is 7-9.

[0014] In some embodiments, the matrix includes cellulose.

[0015] In some embodiments, the matrix includes one or more of microcrystalline cellulose, methyl cellulose, ethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose and carboxymethyl cellulose.

[0016] In some embodiments, the matrix includes one or two of microcrystalline cellulose, hydroxypropyl methylcellulose and carboxymethyl cellulose.

[0017] In some embodiments, the matrix comprises microcrystalline cellulose.

[0018] In some embodiments, the nicotine salt includes one or more of nicotine acetate, nicotine formate, nicotine malate, nicotine benzoate, nicotine citrate, nicotine monotartrate, nicotine bitartrate, nicotine cinnamate, nicotine lactate and nicotine sorbitan salt.

[0019] In some embodiments, during the synthesis of the nicotine salt, the molar ratio of nicotine to organic acid is about 1:1.01 to 1:1.30.

[0020] In some embodiments, during the synthesis of the nicotine salt, the molar ratio of nicotine to organic acid is about 1:1.01 to 1:1.20.

[0021] In some embodiments, the mass ratio of the free nicotine to the nicotine salt is about 1:(2.5-3).

[0022] In some embodiments, the Quercus variabilis and the Licorice are each independently in the form of granules or powder.

[0023] In some embodiments, the mass ratio of the licorice to the free nicotine is about (3-9):1.

[0024] In some embodiments, the ratio of the mass of the plug to the total mass of the free nicotine and the nicotine ions in the nicotine salt is about (2-8):1.

[0025] In some embodiments, the additives include, by weight, about 0.3% to about 3.5% of a binder, about 5% to about 21% of a flavoring agent, about 1% to about 10% of a wetting agent, about 5% to about 30% of a flavoring agent, and about 0.5% to about 3% of a sweetener, based on the product.

[0026] In some embodiments, the binder includes one or more of xanthan gum, gum arabic, sodium alginate, gelatin, starch, pectin, guar gum, tamarind gum and chitosan.

[0027] In some embodiments, the adhesive includes one or more of sodium alginate, gum arabic and starch.

[0028] In some embodiments, the flavoring agent includes one or more of xylitol, sorbitol, maltitol, isomalt, erythritol and D-mannitol.

[0029] In some embodiments, the flavoring agent includes one or more combinations of xylitol, sorbitol, and D-mannitol.

[0030] In some embodiments, the wetting agent includes one or more of propylene glycol, glycerol, and medium chain triglycerides.

[0031] In some embodiments, the flavoring agent includes one or more of natural flavors and synthetic flavors.

[0032] In some embodiments, the sweetener includes one or more of sucralose, acesulfame potassium, neotame, cyclamate, stevia, glycyrrhizin and aspartame.

[0033] In some embodiments, the sweetener includes one or more of sucralose, acesulfame potassium, and neotame.

[0034] In some embodiments, the product is in powder form or granular form.

[0035] In a second aspect, an oral nicotine product is provided, comprising a guanara extract, a base, cork oak, licorice, water, and additives.

[0036] In a third aspect, a method for preparing an oral nicotine product containing free nicotine and nicotine salts is provided, comprising the following steps:

[0037] Step 1: weigh the raw materials according to their weight ratio and set aside;

[0038] Step 2: Mix the powdered ingredients in step 1, licorice, flavoring agent, and binder in a blender to form a mixed matrix material, then add water, continue stirring, mix evenly, and set aside;

[0039] Step 3: Mix free nicotine, nicotine salt, flavor, sweetener, and wetting agent to form a mixed solution, then add cork oak, stir and mix evenly, and set aside;

[0040] Step 4: Add the materials from step 2 to a blender, add the mixed materials from step 3 while stirring, mix well, and then sieve the mixture;

[0041] Step 5: bagging the material from step 4, with each bag containing about 500 mg to about 1000 mg of material. DETAILED DESCRIPTION

[0042] The following will be combined with the embodiments of the present application to clearly and completely describe the technical solutions of the present application. Obviously, the embodiments described are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments of the present application, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of this application.

[0043] In this document, oral nicotine products, nicotine snus products, nicotine snus, and snus products have the same meaning and can be used interchangeably.

[0044] A first aspect of the present application provides an oral nicotine product containing free nicotine and nicotine salts, which includes the following raw materials: free nicotine, nicotine salts, a matrix, cork oak, licorice, water, and additives.

[0045] The nicotine salts in the oral nicotine products of the present application are physically and chemically stable under storage conditions. During the synthesis of the nicotine salts, the molar ratio of nicotine to organic acid is 1:1.01 to 1:1.30. In some embodiments, the molar ratio of nicotine to organic acid is 1:1.01 to 1:1.20. Nicotine salts include, but are not limited to, one or more of nicotine acetate, nicotine formate, nicotine malate, nicotine benzoate, nicotine citrate, nicotine monotartrate, nicotine bitartrate, nicotine cinnamate, nicotine lactate, and nicotine tartrate. When multiple nicotine salts are selected, they can be mixed in any mass ratio. It is understood that during the synthesis of the nicotine salts, the corresponding organic acids include, but are not limited to, one or more of acetic acid, formic acid, malic acid, benzoic acid, citric acid, monotartaric acid, bitartrate, cinnamic acid, lactic acid, and tartrate.

[0046] In some embodiments, in the nicotine salt, nicotine ions account for 40% by weight of the nicotine salt.

[0047] The buccal tobacco product of the present application uses a compounding method of free (free radical) nicotine and nicotine salt. On the one hand, compared with pure free nicotine products, the compounded nicotine buccal tobacco of the present application can reduce the throat irritation caused by free nicotine to the user's oral cavity. At the same time, the performance of the compounded nicotine product is more stable, which is conducive to the transportation and storage of the product. On the other hand, compared with pure nicotine salt products, the compounded nicotine buccal tobacco of the present application can appropriately slow down the release rate of nicotine in the oral mucosa, thereby improving the user's long-term release experience.

[0048] In some embodiments, the mass ratio of free nicotine to nicotine salt in the oral nicotine product is 1:(2.5-3). For example, the mass ratio of free nicotine to nicotine salt in the oral nicotine product is 1:2.5 or 1:3.

[0049] In some embodiments, the mass ratio of free nicotine to nicotine ions in a nicotine salt in an oral nicotine product is 1:(1-1.2). For example, the mass ratio of free nicotine to nicotine ions in a nicotine salt in an oral nicotine product is 1:1 or 1:1.2.

[0050] In some embodiments, the matrix in the present application includes cellulose and cellulose derivatives. In some embodiments, the matrix includes one or more of methylcellulose, ethylcellulose, hydroxypropyl cellulose, hydroxypropyl methylcellulose, and carboxymethyl cellulose. In some embodiments, the matrix includes a combination of one or more of hydroxypropyl methylcellulose and carboxymethyl cellulose, and the multiple combinations can be combined in any mass ratio. In some embodiments, the matrix includes microcrystalline cellulose. Microcrystalline cellulose is a high-quality food and pharmaceutical matrix additive that is inexpensive and can effectively reduce material costs.

[0051] Compared with traditional oral tobacco products, the nicotine oral tobacco products of the present application also contain cork oak. The use of cork oak does not replace the cellulose in traditional nicotine oral tobacco products, but takes advantage of the characteristics of cork oak, such as good liquid adsorption performance, soft texture, good chewing comfort, and excellent stable release performance. Cork oak can absorb the free nicotine and nicotine salts compounded in the present application, as well as additives such as edible flavors and sweeteners, so that when consumers use the oral tobacco products of the present application, the nicotine in the product can be released continuously and stably, effectively improving the duration of the single product experience. Compared with the traditional oral tobacco products that increase the duration of the single product experience by increasing the nicotine or nicotine salt content but sacrificing the experience, the nicotine oral tobacco products of the present application can greatly improve the user's experience time without increasing the nicotine content, keeping the user's experience stable and comfortable. On the other hand, cork oak's soft and elastic texture can significantly improve the mouthfeel of microcrystalline cellulose-based products, enhancing their delicate chewing experience and further increasing their palate comfort. Furthermore, the addition of cork oak can improve product fluidity, significantly increasing mixing and sieving efficiency during the production process, boosting production efficiency and reducing costs.

[0052] In some embodiments, the cork oak may be in the form of granules (with an average particle size of 20-50 mesh) or powder (with an average particle size of 50-200 mesh).

[0053] The preparation process of cork oak particles or powder is as follows: take the branches and trunks of cork oak, remove the cork oak bark, dry and grind them separately, the mass ratio of cork oak trunk to cork oak bark is 1: (2-3), and then sieve.

[0054] In some embodiments, the cork oak comprises cork oak trunk and cork oak bark in a mass ratio of 1:(2-3).

[0055] At the same time, since the bark of the cork oak is colored, for some consumers who do not like colored oral tobacco products, the bark of the cork oak of the present application can also be ground and then added with 20% (mass) hydrogen peroxide + 10% (mass) sodium hypochlorite solution for soaking and rinsing for 30-60 minutes, and then stirred, rinsed and filtered with 60°C warm water, rinsed back and forth three times, and finally dried at 60-80°C.

[0056] In some embodiments, the ratio of the mass of the plug-spark to the total mass of the nicotine ions in the free nicotine and the nicotine salt is (2-8):1. For example, the ratio of the mass of the plug-spark to the total mass of the nicotine ions in the free nicotine and the nicotine salt can be, but is not limited to, 2:1, 4:1, 6:1, 8:1, or a range consisting of any two of these values.

[0057] The nicotine buccal tobacco products of the present application also contain licorice. Compared to traditional nicotine buccal tobacco products that require the addition of large amounts of sweeteners, flavorings, and other additives, the buccal tobacco products of the present application utilize the polysaccharides and aromatic hydrocarbons inherent in licorice to reduce the amount of sweeteners and flavorings used. For low-sugar and low-flavor products demanded by consumers, it is even possible to omit the addition of sweeteners, flavorings, and other additives, and only add licorice. In addition, licorice contains triterpenes, flavonoids, alkaloids, amino acids, and minerals such as Zn, Ca, Sr, Ni, Mn, Fe, Cu, and Cr. In addition to its effects of tonifying the spleen and replenishing qi, moistening the lungs and relieving coughs, clearing away heat and detoxifying, and harmonizing various medicines, it is also used to treat symptoms such as sore throat, spleen and stomach deficiency and cold, peptic ulcers, and poisoning. After consuming the nicotine product, the user continues to chew the product of the present application, allowing the aforementioned substances in the licorice to be absorbed through the mouth, improving the oral environment and reducing the user's oral morbidity. In addition, the addition of licorice in this application can significantly reduce the spicy sensation in the throat caused by the compound nicotine-nicotine salt, thereby improving the eating comfort of the product.

[0058] Licorice can be in the form of granules (average particle size of 20-50 meshes) or powder (average particle size of 50-200 meshes). The preparation process of licorice granules or powder is as follows: remove the leaves and skin of licorice, dry it and grind it.

[0059] In some embodiments, the mass ratio of licorice to free nicotine is (3-9): 1. For example, the mass ratio of licorice to free nicotine is 3:1, 5:1, 7:1, 9:1, or a range consisting of any two of these values.

[0060] The oral tobacco product of the present application can be in powder form or granular form. The average particle size of the granular form is 20 mesh to 50 mesh. The licorice or cork oak raw material can be in powder form or granular form. If the oral tobacco product of the present application needs to be made into a powder form (average particle size greater than 50 mesh), the licorice or cork oak raw material is in powder form.

[0061] In order to meet the needs of different consumers, for consumers who have a high demand for additives that improve the taste, such as sweetness and fragrance, the additives in the nicotine oral tobacco product of the present application include one or more of a binder, a flavoring agent, a wetting agent, a flavoring agent and a sweetener.

[0062] In some embodiments, the binder is a natural binder. The binder includes one or more combinations of xanthan gum, gum arabic, sodium alginate, gelatin, starch, pectin, guar gum, tamarind gum, and chitosan. When multiple combinations are selected, they can be mixed in any mass ratio.

[0063] In some embodiments, the binder includes one or more of sodium alginate, gum arabic, and starch.

[0064] In some embodiments, the flavoring agent comprises a sugar alcohol. The flavoring agent comprises one or more of xylitol, sorbitol, maltitol, isomalt, erythritol, D-mannitol, etc. In some embodiments, the flavoring agent comprises one or more combinations of xylitol, sorbitol, and D-mannitol. When selecting multiple combinations, any mass ratio can be used.

[0065] In some embodiments, the wetting agent includes one or more combinations of propylene glycol, glycerol, and medium-chain triglycerides. When multiple combinations are selected, they can be mixed in any mass ratio.

[0066] In some embodiments, flavoring agents include natural and synthetic flavors.

[0067] In some embodiments, the sweetener includes one or more combinations of sucralose, acesulfame potassium, neotame, cyclamate, stevia, glycyrrhizin, and aspartame. When multiple combinations are selected, they can be blended in any mass ratio. In some embodiments, the sweetener includes one or more of sucralose, acesulfame potassium, and neotame.

[0068] In some embodiments, the pH of the oral nicotine product of the present application is 7-9.

[0069] In order to better control the pH of the oral nicotine product of the present application within the range of 7-9, a small amount of pH adjuster may be added to the components of the present application. The specific amount added is preferably such that the pH of the oral nicotine product is adjusted to 7-9.

[0070] The oral nicotine product of the present application comprises, by mass percentage, 0.3%-4% free nicotine, 0.75%-10% nicotine salt, 20%-50% matrix, 3%-20% cork oak, 2%-10% licorice, 5%-30% water, and the remainder being additives; the pH is 7-9.

[0071] The additives, calculated by mass percentage, include 0.3%-3.5% of a binder, 5%-21% of a flavoring agent, 1%-10% of a wetting agent, 5%-30% of a flavoring agent, and 0.5%-3% of a sweetener.

[0072] In some embodiments, the free nicotine and nicotine salts can be replaced with guanara extract. That is, the oral tobacco product includes guanara extract, a base, cork oak, licorice, water, and additives.

[0073] Beneficial effects of this application:

[0074] 1. By compounding free nicotine and nicotine salts, the compounded nicotine buccal tobacco product of the present application can reduce the spicy sensation of nicotine buccal tobacco products compared to pure free nicotine buccal tobacco products. At the same time, compared to buccal tobacco products that only use nicotine salt products, the buccal tobacco of the present application can increase the release time of nicotine in the oral cavity.

[0075] 2. By adding licorice to the product, the present application not only reduces the throat hit of nicotine and enhances the mouthfeel of the snus product, but also utilizes the inherent sweetness of licorice to reduce the use of flavoring agents and sweeteners. Furthermore, licorice can improve the oral environment and reduce oral morbidity in users.

[0076] 3. The buccal tobacco product of the present application, by adding cork oak to the raw materials, can, on the one hand, allow the cork oak to absorb nicotine, significantly increasing the duration of nicotine release in the user's mouth, extending the experience of the single product, and making it more likely to gain consumer favor. Furthermore, the addition of cork oak can improve the chewing performance of the buccal tobacco product of the present application, making the chewing experience more chewy and comfortable. Furthermore, the addition of cork oak can improve the fluidity of the product, greatly improving the stirring and sieving efficiency during the production process, improving production efficiency, and reducing production costs.

[0077] A second aspect of the present application provides a method for preparing an oral nicotine product, comprising the following steps:

[0078] Step 1: weigh the raw materials according to the above weight ratio;

[0079] Step 2: Mix the powdered raw materials such as cellulose, licorice, flavoring agent, binder, and pH adjuster in a blender to form a mixed matrix material, then add water, continue stirring, and set aside;

[0080] Step 3: Mix free nicotine, nicotine salt, flavor, sweetener, and wetting agent to form a mixed solution, then add cork oak, stir and mix evenly, and set aside;

[0081] Step 4: Add the material from step 2 to a blender, add the mixed material from step 3 while stirring, mix evenly, and then sieve the mixture. You can dry it according to actual needs.

[0082] Step 5: bag the material from step 4, with 500mg-1000mg of material in each bag.

[0083] The present application is described below with reference to examples with different proportions.

[0084] Example 1

[0085] The oral tobacco product of Example 1 of the present application comprises, by mass percentage, 0.3% free nicotine, 0.75% nicotine salt, 20% base, 3% cork oak, 2% licorice, 9.65% water, 0.3% binder, 21% flavoring agent, 10% wetting agent, 30% flavoring agent, and 3% sweetener.

[0086] Example 2

[0087] The oral tobacco product of Example 2 of the present application comprises, by mass percentage, 1% free nicotine, 2.5% nicotine salt, 32.5% base, 8% cork oak, 5% licorice, 10% water, 1% binder, 18% flavoring agent, 6% wetting agent, 15% flavoring agent, and 1% sweetener.

[0088] Example 3

[0089] The oral tobacco product of Example 3 of the present application comprises, by mass percentage, 1% free nicotine, 3% nicotine salt, 50% base, 5% cork oak, 4% licorice, 11% water, 1% binder, 8% flavoring agent, 6% wetting agent, 10% flavoring agent and 1% sweetener.

[0090] Example 4

[0091] The oral tobacco product of Example 4 of the present application comprises, by mass percentage, 2% free nicotine, 5% nicotine salt, 34% matrix, 5% cork oak, 3% licorice, 30% water, 1% binder, 8% flavoring agent, 1% wetting agent, 10% flavoring agent, and 1% sweetener.

[0092] Example 5

[0093] The oral tobacco product of Example 5 of the present application comprises, by mass percentage, 4% free nicotine, 10% nicotine salt, 20% base, 20% cork oak, 10% licorice, 17% water, 3.5% binder, 5% flavoring agent, 5% wetting agent, 5% fragrance, and 0.5% sweetener.

[0094] Example 6

[0095] The oral tobacco product of Example 6 of the present application comprises, by mass percentage, 1% free nicotine, 2.5% nicotine salt, 34.5% base, 8% cork oak, 3% licorice, 10% water, 1% binder, 18% flavoring agent, 6% wetting agent, 15% flavoring agent, and 1% sweetener.

[0096] Example 7

[0097] The oral tobacco product of Example 7 of the present application comprises, by mass percentage, 1% free nicotine, 2.5% nicotine salt, 30.5% base, 8% cork oak, 7% licorice, 10% water, 1% binder, 18% flavoring agent, 6% wetting agent, 15% flavoring agent, and 1% sweetener.

[0098] Example 8

[0099] The oral tobacco product of Example 8 of the present application comprises, by mass percentage, 1% free nicotine, 2.5% nicotine salt, 28.5% base, 8% cork oak, 9% licorice, 10% water, 1% binder, 18% flavoring agent, 6% wetting agent, 15% flavoring agent, and 1% sweetener.

[0100] Example 9

[0101] The oral tobacco product of Example 9 of the present application comprises, by mass percentage, 1% free nicotine, 2.5% nicotine salt, 36.5% base, 4% cork oak, 5% licorice, 10% water, 1% binder, 18% flavoring agent, 6% wetting agent, 15% fragrance, and 1% sweetener.

[0102] Example 10

[0103] The oral tobacco product of Example 10 of the present application comprises, by mass percentage, 1% free nicotine, 2.5% nicotine salt, 28.5% base, 12% cork oak, 5% licorice, 10% water, 1% binder, 18% flavoring agent, 6% wetting agent, 15% flavoring agent, and 1% sweetener.

[0104] Example 11

[0105] The oral tobacco product of Example 11 of the present application comprises, by mass percentage, 1% free nicotine, 2.5% nicotine salt, 24.5% base, 16% cork oak, 5% licorice, 10% water, 1% binder, 18% flavoring agent, 6% wetting agent, 15% flavoring agent, and 1% sweetener.

[0106] In Examples 1-11, the nicotine salt is tartrate, the matrix is ​​microcrystalline cellulose, the binder is sodium alginate, the flavoring agent is maltitol, the flavoring agent is natural flavor, and the sweetener is acesulfame potassium.

[0107] In the above examples, the additives, free nicotine, and nicotine salt contents in Example 2 and Examples 6-11 are the same, and thus can be used as reference examples for evaluation.

[0108] Comparative Example 12

[0109] The oral tobacco product of Comparative Example 12 is similar to that of Example 2, except that the cork oak in Example 2 is replaced by a matrix of microcrystalline cellulose, that is, Comparative Example 12 does not contain cork oak.

[0110] Comparative Example 13

[0111] The oral tobacco product of Comparative Example 13 is similar to that of Example 2, except that the licorice in Example 2 is replaced by a matrix of microcrystalline cellulose, that is, Comparative Example 13 does not contain licorice.

[0112] Comparative Example 14

[0113] The oral tobacco product of Comparative Example 14 is similar to that of Example 2, except that the licorice and cork oak in Example 2 are replaced by a matrix of microcrystalline cellulose, that is, Comparative Example 14 does not contain licorice and cork oak.

[0114] Comparative Example 15

[0115] The oral tobacco product of Comparative Example 15 is similar to that of Example 2, except that the free nicotine in Example 2 is replaced by a matrix of microcrystalline cellulose, that is, Comparative Example 15 does not contain free nicotine.

[0116] Comparative Example 16

[0117] The oral tobacco product of Comparative Example 16 is similar to that of Example 2, except that the nicotine salt in Example 2 is replaced by a matrix of microcrystalline cellulose, that is, Comparative Example 16 does not contain nicotine salt.

[0118] Comparative Example 17

[0119] The oral tobacco product of Comparative Example 17 is similar to Comparative Example 15, except that the licorice and cork oak in Comparative Example 15 are replaced with a matrix of microcrystalline cellulose, that is, Comparative Example 17 does not contain free nicotine, licorice, and cork oak.

[0120] Comparative Example 18

[0121] The oral tobacco product of Comparative Example 18 is similar to Comparative Example 16, except that the licorice and cork oak in Comparative Example 16 are replaced with a matrix of microcrystalline cellulose, that is, Comparative Example 18 does not contain nicotine salt, licorice, and cork oak.

[0122] Performance Testing

[0123] The following comparative experiments were conducted to evaluate the release rate, taste stimulation and taste duration, fluidity, and elasticity of the oral tobacco products prepared in Examples 2, 6-11, Comparative Examples 12, 13, 14, 15, 16, 17, and 18, the existing patented technology (patent application number: 201280017683.0, the product prepared in Example 1-J, which is a nicotine salt oral tobacco product), and the commercially available oral tobacco products (which are free nicotine oral tobacco products).

[0124] Evaluation test methods

[0125] Example 2, Examples 6-11, Comparative Examples 12-18, and Example 1-J of the prior art were made into bagged products (500 mg / bag) identical to commercially available products. Ten bags of each test sample were prepared and distributed to 10 subjects. The testers placed the snus sample between the gums and the inner mucosa of the lips, and the testers' sense of irritation to the mucosa, the time required to feel the physiological effects of nicotine, and the time it took for the physiological effects of nicotine to disappear were recorded.

[0126] The irritation of the mucous membrane was scored from 1 to 20 points from weak to strong;

[0127] The time to start feeling the physiological effects of nicotine stimulation (stimulation time) is calculated from the time the test subject puts the snus into the mouth, in seconds;

[0128] The time to lose the physiological effect of nicotine stimulation (release duration) is calculated from the time the tester puts the snus into the mouth, in seconds;

[0129] After removing the maximum and minimum test results for each test result, the remaining eight groups of results were averaged. The test results are shown in Table 2.

[0130] Table 1 Main raw materials of Example 2, Examples 6-11, and Comparative Examples 12-18 (mass percentage)

[0131] In Table 1, “-” indicates that the component is not contained.

[0132] Since the nicotine ion content in nicotine salt only accounts for about 40% of the total weight of nicotine salt, in each 500 mg sample in Examples 2 and Examples 6-11 of the present application, the nicotine salt content is 2.5%, the mass percentage of nicotine ions is 1%, and the nicotine ion content in the nicotine salt is 5 mg.

[0133] Table 2 Test results of various embodiments and comparative examples

[0134] Analyzing the above stimulation results, we can know that:

[0135] 1. By comparing the irritation test results of the existing patented product, Comparative Example 17, and the commercially available product, Comparative Example 18, it can be seen that the throat irritation of the oral tobacco product containing free nicotine is significantly stronger than the throat irritation of the nicotine salt oral tobacco product, indicating that in oral tobacco products, the throat irritation experience mainly comes from free nicotine, which is consistent with theory.

[0136] 2. It can be seen from the results of Comparative Examples 13 and 14 in Table 2 that simply adding cork oak to the oral smoke product cannot improve the throat irritation of the product; further, by comparing the irritation test results of Example 2, Examples 6-11, Comparative Examples 12, Comparative Example 15, Comparative Example 16 with Comparative Example 13, Comparative Example 14, Comparative Example 18, and commercially available products, it can be seen that the present application can effectively reduce the irritation of nicotine to the oral cavity by adding licorice to the oral smoke product and improve the user experience. By comparing the throat irritation results of Example 2, Example 6, Example 7, and Example 8, it can be seen that by adjusting the amount of licorice added to the oral smoke product, it is beneficial to adjust the throat irritation of nicotine in the oral smoke product and improve the taste comfort of the oral smoke.

[0137] 3. By comparing the irritation test results of Examples 2 and 6-11 with Comparative Examples 13 and 14, it can be seen that when the total nicotine content in the materials is the same, the inclusion of licorice in Examples 2 and 6-11 can significantly reduce the throat irritation of nicotine, thereby improving the taste comfort of the products.

[0138] 4. By comparing the stimulation test results of Examples 2 and 6-11 with those of the existing patented technology and commercially available products, it can be seen that even though the total nicotine content in the products prepared in Examples 2 and 6-11 of the present application is greater than that in the existing patented technology and commercially available products, the addition of licorice can still significantly reduce the throat irritation of the products. The throat irritation of the products is even better than that of the existing patented technology oral tobacco products that only add nicotine salts.

[0139] Analysis of the above stimulation start time results shows that:

[0140] 1. A comparative analysis of the stimulation time of Comparative Example 17, the existing patented product, and Comparative Example 18, the commercially available product, shows that the oral diffusion rate of the snus product containing nicotine salt is significantly faster than that of the snus product containing free nicotine, which is consistent with theory.

[0141] 2. Analysis of the stimulation time results for Example 2, Examples 6-11, Comparative Examples 12-15, and Comparative Example 17 shows that as long as the snus product contains nicotine salt, the stimulation time in the oral cavity does not differ significantly. The nicotine salt content in the product is not significantly different, and the onset time of stimulation in the oral cavity does not differ significantly.

[0142] Analyzing the above release duration results, we can see that:

[0143] 1. By comparing the release duration results of Comparative Example 13 with Comparative Examples 12 and 14, it can be seen that by adding Quercus variabilis to a snus product, the release duration of the snus product in the oral cavity can be significantly increased. Further, by analyzing the release duration results of Comparative Examples 15 and 16 with Comparative Examples 17 and 18, existing products, and commercially available products, it can be seen that in snus products, even when the nicotine content is the same, by adding Quercus variabilis to the snus, the release duration of the snus product in the oral cavity can still be significantly increased, thereby improving the experience duration of the single product. By comparing the results of Comparative Examples 15 and 16 with Comparative Example 14, it can be seen that even if the total nicotine content in the products of Comparative Examples 15 and 16 is less than the total nicotine content in Comparative Example 14, the addition of Quercus variabilis can still significantly increase the release duration of the snus products of Comparative Examples 15 and 16 in the user's oral cavity.

[0144] 2. The release duration results of Examples 2, 9, 10, and 11 show that as the Quercus variabilis content in the snus product increases, the release duration of nicotine in the oral cavity increases accordingly, but the subsequent increase decreases.

[0145] 3. By comparing the release duration results of Examples 2 and 6-11 with existing patented technologies and commercially available products, combined with the above-mentioned Conclusions 1 and 2, it can be seen that the oral tobacco products of the present application, by adding cork oak to the oral tobacco raw materials and combining them with other components, can significantly increase the release duration of nicotine in the product in the oral cavity, thereby improving the experience time of the single product.

[0146] Liquidity test

[0147] Evaluation objects: Example 2, Comparative Example 12, Comparative Example 13, Comparative Example 14, traditional technology products, commercially available products

[0148] Evaluation Method: Using a conical funnel with a 100mm opening and a 10mm inner diameter, pour 15g of prepared granular or powdered material continuously (5 seconds) along the edge of the opening into the funnel. Measure the time it takes for the material to flow out of the funnel. Ten replicates are tested for each sample, and the average result is taken. Sample flowability is expressed as mass flow rate, using the formula: mass flow rate = sample mass / time required for flow. See Table 3 for test results.

[0149] Table 3 Fluidity test results of oral tobacco products

[0150] It can be seen from the results of Comparative Examples 12, 13 and 14 that the addition of cork oak to the buccal tobacco product can significantly improve the fluidity of the product, facilitate stirring and mixing during the production process, and reduce production costs. The test results of Example 2, conventional technology products and commercially available products show that the buccal tobacco product of the present application has better fluidity than conventional technology products and commercially available products by adding cork oak and coordinating with other components.

[0151] Elasticity test

[0152] Evaluation objects: Example 2, Comparative Example 12, Comparative Example 13, Comparative Example 14, traditional technology products, and commercially available products.

[0153] Evaluation Methodology

[0154] An acrylic plate trough with scale marks on the side was used. The length, width, and depth of the acrylic plate trough were 2cm, 1cm, and 5cm respectively. 30g of each sample was poured into the trough and spread flat. The scale was recorded. Then, an I-shaped piston was used to cover the trough. A 500g weight was applied to the piston. After 10 minutes, the scale was recorded. The I-shaped piston was then removed and the scale was recorded again after 10 minutes. Ten test samples were taken for each evaluation object, and the test results were averaged. The test results are as follows:

[0155] Table 4 Elasticity test results of oral tobacco products

[0156] By comparing the flattening scale data of Example 2 and Comparative Example 13 with the data of other test samples, it can be seen that adding Quercus variabilis to the snus product, in combination with other components, can make the snus product fluffier. At the same time, the rebound data shows that adding Quercus variabilis to the sample, in combination with other components, can significantly enhance the resilience of the snus product, improve the chewing resistance of the snus product, and enhance the taste comfort.

[0157] In summary, the above test results show that:

[0158] 1. By compounding free nicotine and nicotine salts, the present application can significantly reduce the spicy sensation of oral tobacco products compared to single free nicotine oral tobacco products. At the same time, compared to oral tobacco products that only use nicotine salt products, the oral tobacco of the present application can significantly increase the release time of nicotine in the oral cavity.

[0159] 2. By adding licorice to the product, the present application can, on the one hand, utilize licorice to suppress the irritation of nicotine hitting the throat and improve the taste comfort of the snus product; on the other hand, by utilizing the sweet and fragrant characteristics of licorice itself, the use of some flavoring agents and sweeteners can be reduced. In addition, licorice can also improve the oral environment and reduce the incidence of oral diseases in users.

[0160] 3. The snus products of the present application, by adding cork oak to the raw materials, can, on the one hand, allow the cork oak to absorb nicotine, significantly increasing the duration of nicotine release in the user's mouth, improving the user experience of the product, and making the product more likely to gain consumer favor. Furthermore, the addition of cork oak to the snus products of the present application can improve the chewing properties of the product, making the chewing experience more chewy and comfortable. Furthermore, the addition of cork oak can improve the fluidity of the product, significantly improving the stirring and sieving efficiency during the production process, thereby improving production efficiency and reducing production costs.

[0161] The technical features of the above-mentioned embodiments can be combined arbitrarily. In order to make the description concise, not all possible combinations of the technical features in the above-mentioned embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0162] The above-described embodiments merely represent several implementation methods of the present application. While the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the patent application. It should be noted that a person of ordinary skill in the art may make various modifications and improvements without departing from the spirit of the present application, and these modifications and improvements fall within the scope of protection of the present application. Therefore, the scope of protection of the present patent application shall be determined by the appended claims.

Claims

1. An oral nicotine product containing free nicotine and nicotine salt, wherein: Includes free nicotine, nicotine salts, base, cork oak, licorice, water and additives.

2. The oral nicotine product containing free nicotine and nicotine salt according to claim 1, wherein: The product comprises, by mass percentage, about 0.3% to about 4% of free nicotine, about 0.75% to about 10% of nicotine salt, about 20% to about 50% of base, about 3% to about 20% of cork oak, about 2% to about 10% of liquorice, about 5% to about 30% of water, and the rest being additives.

3. The oral nicotine product containing free nicotine and nicotine salt according to claim 1 or 2, wherein: The pH of the preparation is 7-9.

4. The oral nicotine product containing free nicotine and nicotine salt according to any one of claims 1 to 3, wherein: The matrix includes cellulose.

5. The oral nicotine product containing free nicotine and nicotine salt according to claim 4, wherein: The matrix includes one or more of microcrystalline cellulose, methyl cellulose, ethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose and carboxymethyl cellulose.

6. The oral nicotine product containing free nicotine and nicotine salt according to claim 5, wherein: The matrix includes one or two of microcrystalline cellulose, hydroxypropyl methylcellulose and carboxymethyl cellulose.

7. The oral nicotine product containing free nicotine and nicotine salt according to claim 6, wherein: The matrix includes microcrystalline cellulose.

8. The oral nicotine product containing free nicotine and nicotine salt according to any one of claims 1 to 7, wherein: The nicotine salt includes one or more of nicotine acetate, nicotine formate, nicotine malate, nicotine benzoate, nicotine citrate, nicotine monotartrate, nicotine bitartrate, nicotine cinnamate, nicotine lactate and nicotine sorbitanate.

9. The oral nicotine product containing free nicotine and nicotine salt according to any one of claims 1 to 8, wherein: During the synthesis of the nicotine salt, the molar ratio of nicotine to organic acid is about 1:1.01 to 1:1.

30.

10. The oral nicotine product containing free nicotine and nicotine salt according to claim 9, wherein: During the synthesis of the nicotine salt, the molar ratio of nicotine to organic acid is about 1:1.01 to 1:1.

20.

11. The oral nicotine product containing free nicotine and nicotine salt according to any one of claims 1 to 10, wherein: The mass ratio of the free nicotine to the nicotine salt is about 1:(2.5-3).

12. An oral nicotine product containing free nicotine and nicotine salt according to any one of claims 1 to 11, wherein: The cork oak and the liquorice are each independently in the form of particles or powder.

13. The oral nicotine product containing free nicotine and nicotine salt according to any one of claims 1 to 12, wherein: The mass ratio of the licorice to the free nicotine is about (3-9):

1.

14. The oral nicotine product containing free nicotine and nicotine salt according to any one of claims 1 to 13, wherein: The ratio of the mass of the plug to the total mass of the free nicotine and the nicotine ions in the nicotine salt is about (2-8):

1.

15. The oral nicotine product containing free nicotine and nicotine salt according to any one of claims 1 to 14, wherein: The additives include one or more of a binder, a flavoring agent, a wetting agent, a fragrance and a sweetener.

16. The oral nicotine product containing free nicotine and nicotine salt according to claim 15, wherein: In terms of mass percentage, the additives include about 0.3% to about 3.5% of a binder, about 5% to about 21% of a flavoring agent, about 1% to about 10% of a wetting agent, about 5% to about 30% of a flavoring agent, and about 0.5% to about 3% of a sweetener.

17. The oral nicotine product containing free nicotine and nicotine salt according to any one of claims 15 to 16, wherein: The adhesive comprises one or more of xanthan gum, gum arabic, sodium alginate, gelatin, starch, pectin, guar gum, tamarind gum and chitosan.

18. The oral nicotine product containing free nicotine and nicotine salt according to claim 17, wherein: The adhesive comprises one or more of sodium alginate, gum arabic and starch.

19. The oral nicotine product containing free nicotine and nicotine salt according to any one of claims 15 to 18, wherein: The flavoring agent includes one or more of xylitol, sorbitol, maltitol, isomalt, erythritol and D-mannitol.

20. The oral nicotine product containing free nicotine and nicotine salt according to claim 19, wherein: The flavoring agent includes one or more combinations of xylitol, sorbitol and D-mannitol.

21. The oral nicotine product containing free nicotine and nicotine salt according to any one of claims 15 to 20, wherein: The wetting agent includes one or more of propylene glycol, glycerol and medium chain triglycerides.

22. The oral nicotine product containing free nicotine and nicotine salt according to any one of claims 15 to 21, wherein: The flavoring agent includes one or more of natural flavors and synthetic flavors.

23. The oral nicotine product containing free nicotine and nicotine salt according to any one of claims 15 to 22, wherein: The sweetener includes one or more of sucralose, acesulfame potassium, neotame, cyclamate, stevioside, glycyrrhizin and aspartame.

24. The oral nicotine product containing free nicotine and nicotine salt according to claim 23, wherein: The sweetener includes one or more of sucralose, acesulfame potassium and neotame.

25. The oral nicotine product containing free nicotine and nicotine salt according to any one of claims 1 to 24, wherein: The product is in powder form or granule form.

26. An oral nicotine product, wherein: Includes guanara extract, base, cork oak, liquorice, water and additives.

27. The oral nicotine product containing free nicotine and nicotine salt according to any one of claims 15 to 25, wherein: The preparation method of the product comprises the following steps: Step 1, weigh each raw material according to the weight ratio of each material and set aside; Step 2, mixing the powdered base, licorice, flavoring agent, and adhesive in a blender to form a mixed base material, then adding water, continuing to stir, mixing evenly, and setting aside; Step 3, mixing free nicotine, nicotine salt, flavor, sweetener, and wetting agent to form a mixed solution, then adding cork oak, stirring and mixing evenly, and setting aside; Step 4, adding the materials of step 2 into a blender, adding the mixed materials of step 3 while blending, mixing evenly, and then sieving the mixture; Step 5, bagging the material from step 4, with each bag containing about 500 mg to about 1000 mg of material.

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