Nicotine-alginate, preparation method thereof and buccal cigarette containing the same

Abstract

The present invention provides a kind of nicotine-alginate, its preparation method and oral cigarette containing it, step 1: obtain alginic acid-ethanol suspension; step 2: obtain nicotine ethyl acetate solution; step 3: add the solution obtained in step 2 dropwise to the suspension obtained in step 1, add dropwise while stirring, obtain alginic acid-nicotine salt solution, concentrate under reduced pressure to remove solvent, obtain brown-yellow viscous liquid, place in refrigerator and stand at low temperature until solid precipitates; step 4: crush the solid obtained in step 3, add to ethyl acetate, stir and filter, and wash the filter cake with ethyl acetate to obtain brown-yellow solid nicotine-alginate. The method of the present invention is simple and reliable, and the obtained solid nicotine-alginate is used in gum-based chewing tobacco and oral cigarette, which can make nicotine more uniform, slow and lasting release in the oral cavity, provide consumers with long-lasting and peaceful physiological satisfaction, and effectively reduce the irritation to the digestive tract.

Description

Technical field:

[0001] The invention belongs to the technical field of tobacco, and relates to a nicotine-alginate, a preparation method thereof and a buccal cigarette containing the same, and is a slow-release solid nicotine salt specially used for buccal cigarettes. Background technology:

[0002] Nicotine is an important component of tobacco and the main component that brings satisfaction and pleasure to tobacco product users. Currently, nicotine used in new tobacco products mostly exists in the form of tobacco extracts, free nicotine, liquid nicotine salts, etc. This will cause the product to release nicotine too quickly and too violently when consumed, causing certain oral and gastrointestinal irritation and causing physical discomfort. Solid nicotine salts are also used in oral cigarettes to reduce the release rate and increase the release time, but due to the special properties of different nicotine salts themselves, the release rate is still fast and the duration is not long enough.

[0003] There is currently no method for preparing nicotine-alginate in solid form, and liquid nicotine salt or other solid nicotine salt is currently used in oral cigarettes.

[0004] The use of liquid nicotine-alginate in new tobacco products causes the nicotine to be released too quickly and too violently when consumed, which can cause certain oral and gastrointestinal irritation and physical discomfort. The release rate of nicotine salts from other organic acids is still too fast and the duration is not long enough. Summary of the invention:

[0005] The purpose of the present invention is to solve the deficiencies of the prior art and to provide a nicotine-alginate, a preparation method thereof and a buccal cigarette containing the nicotine-alginate.

[0006] The preparation method is simple and reliable. The prepared solid nicotine-alginate is used in gum-based chewing tobacco and buccal tobacco, which can release nicotine more evenly, slowly and lastingly in the oral cavity, providing consumers with long-lasting and peaceful physiological satisfaction, while effectively reducing irritation to the digestive tract.

[0007] The object of the present invention is achieved in that:

[0008] A method for preparing nicotine-alginate, comprising the following steps:

[0009] Step 1: Add alginate to a certain amount of ethanol and stir to completely swell it to obtain an alginate-ethanol suspension;

[0010] Step 2: Add nicotine to a certain amount of ethyl acetate, stir to clarify, and obtain a nicotine ethyl acetate solution;

[0011] Step 3: Add the ethyl acetate solution of nicotine obtained in step 2 dropwise to the alginate-ethanol suspension obtained in step 1, while stirring. After the addition is complete, stir at room temperature for 3-5 hours to obtain an alginate-nicotine salt solution, and concentrate under reduced pressure to remove the solvent to obtain a brown-yellow viscous liquid, which is placed in a refrigerator and refrigerated for 3-7 days until solids precipitate;

[0012] Step 4: Crush the solid obtained in step 3, add it to a certain amount of ethyl acetate, stir for 16 hours, filter, wash the filter cake with ethyl acetate 2-3 times to obtain a brown solid, and dry the obtained brown solid in vacuo at 50-75°C to obtain brown solid nicotine-alginate.

[0013] The present invention also includes the following technical features:

[0014] 1. The molar ratio of nicotine to alginic acid is 1:(0.7-1.1), preferably 1:(0.8-0.95).

[0015] 2. The ethanol added in step 1 is 1-8 times the mass of the alginate, preferably 3-5 times.

[0016] 3. The amount of ethyl acetate used in step 2 is 1-8 times, preferably 3-5 times, the mass of nicotine.

[0017] 4. In step 4, the mass of ethyl acetate is 10-50 times that of alginate, preferably 20-30 times.

[0018] 5. In step 4, the ethyl acetate used for washing the filter cake each time is 1-8 times the mass of alginate, preferably 3-5 times.

[0019] 6. The vacuum drying temperature is 40-85°C, preferably 60-75°C.

[0020] The present invention also provides a nicotine-alginate prepared by any one of the above methods.

[0021] The present invention also provides a nicotine-alginate oral cigarette, which is prepared by the following method: preparing materials: 5% nicotine-alginate, 65% microcrystalline cellulose, and 5% propylene glycol; mixing and sieving the materials, taking powder particles with a particle size of 20 mesh and mixing them evenly, respectively baking and heating in a pasteurizer, adding 10% water, 3% sodium chloride, and 2% sodium carbonate, blending evenly, refrigerating for 12 hours, spraying 4% honey, 4% glucose, 1% aspartame, and 1% vitamin E, sealing and refrigerating for 24 hours, sterilizing by ultraviolet for 3 hours, and packaging to obtain the finished product.

[0022] The present invention also provides a method for preparing a nicotine-alginate oral cigarette, comprising the steps of preparing materials: 5% nicotine-alginate, 65% microcrystalline cellulose and 5% propylene glycol; mixing and sieving the materials, taking powder particles with a particle size of 20 mesh and mixing them evenly, respectively baking and heating in a pasteurizer, adding 10% water, 3% sodium chloride and 2% sodium carbonate, blending them evenly, refrigerating them for 12 hours, spraying 4% honey, 4% glucose, 1% aspartame and 1% vitamin E, sealing and refrigerating them for 24 hours, sterilizing them with ultraviolet light for 3 hours, and packaging them into finished products.

[0023] Compared with the prior art, the present invention has the following beneficial effects:

[0024] The present invention relates to the technical field of chemical synthesis, and in particular to a method for preparing nicotine-alginate. The method for preparing nicotine-alginate provided by the present invention uses ethanol and ethyl acetate as reaction solvents and purification solvents; the method is simple and easy to operate, has low production cost, high product salinity, and is suitable for industrialized scale-up production; the obtained solid is a uniform brown-yellow powder, and the solid color and state are relatively good, and it is applied to new tobacco such as buccal cigarettes, and is easy to use. Description of the drawings:

[0025] Figure 1 The solid nicotine-alginate prepared by the present invention;

[0026] Figure 2 This is the nicotine release curve of nicotine-alginate snus. Specific implementation method:

[0027] At present, there are few studies on solid nicotine-alginate, and a method for preparing solid nicotine-alginate has not been found. The present invention uses ethanol and ethyl acetate as solvents, reacts at room temperature for 4-6 hours, concentrates to remove ethanol and ethyl acetate after the reaction, and solidifies by standing at low temperature, then crushes, adds ethyl acetate for pulping, washes, purifies, filters, and vacuum dries to obtain brown-yellow powder with good properties and convenient use.

[0028] A method for preparing nicotine-alginate, comprising the following steps:

[0029] Step 1: Add alginate to a certain amount of ethanol and stir to completely swell it to obtain an alginate-ethanol suspension;

[0030] Step 2: Add nicotine to a certain amount of ethyl acetate, stir to clarify, and obtain a nicotine ethyl acetate solution;

[0031] Step 3: Add the ethyl acetate solution of nicotine obtained in step 2 dropwise to the alginate-ethanol suspension obtained in step 1, while stirring. After the addition is complete, stir at room temperature for 3-5 hours to obtain an alginate-nicotine salt solution, and concentrate under reduced pressure to remove the solvent to obtain a brown-yellow viscous liquid, which is placed in a refrigerator and refrigerated for 3-7 days until solids precipitate;

[0032] Step 4: Crush the solid obtained in step 3, add it to a certain amount of ethyl acetate, stir for 16 hours, filter, wash the filter cake with ethyl acetate 2-3 times to obtain a brown solid, and dry the obtained brown solid in vacuo at 50-75°C to obtain brown solid nicotine-alginate.

[0033] The present invention also includes the following technical features:

[0034] 1. The molar ratio of nicotine to alginic acid is 1:(0.7-1.1), preferably 1:(0.8-0.95).

[0035] 2. The ethanol added in step 1 is 1-8 times the mass of the alginate, preferably 3-5 times.

[0036] 3. The amount of ethyl acetate used in step 2 is 1-8 times, preferably 3-5 times, the mass of nicotine.

[0037] 4. In step 4, the mass of ethyl acetate is 10-50 times that of alginate, preferably 20-30 times.

[0038] 5. In step 4, the ethyl acetate used for washing the filter cake each time is 1-8 times the mass of alginate, preferably 3-5 times.

[0039] 6. The vacuum drying temperature is 40-85°C, preferably 60-75°C.

[0040] The present invention also provides a nicotine-alginate prepared by any one of the above methods.

[0041] The present invention also provides a nicotine-alginate oral cigarette, which is prepared by the following method: preparing materials: 5% nicotine-alginate, 65% microcrystalline cellulose, and 5% propylene glycol; mixing and sieving the materials, taking powder particles with a particle size of 20 mesh and mixing them evenly, respectively baking and heating in a pasteurizer, adding 10% water, 3% sodium chloride, and 2% sodium carbonate, blending evenly, refrigerating for 12 hours, spraying 4% honey, 4% glucose, 1% aspartame, and 1% vitamin E, sealing and refrigerating for 24 hours, sterilizing by ultraviolet for 3 hours, and packaging to obtain the finished product.

[0042] The present invention also provides a method for preparing a nicotine-alginate oral cigarette, comprising the steps of preparing materials: 5% nicotine-alginate, 65% microcrystalline cellulose and 5% propylene glycol; mixing and sieving the materials, taking powder particles with a particle size of 20 mesh and mixing them evenly, respectively baking and heating in a pasteurizer, adding 10% water, 3% sodium chloride and 2% sodium carbonate, blending them evenly, refrigerating them for 12 hours, spraying 4% honey, 4% glucose, 1% aspartame and 1% vitamin E, sealing and refrigerating them for 24 hours, sterilizing them with ultraviolet light for 3 hours, and packaging them into finished products.

[0043] Embodiment 1:

[0044] Prepare the materials according to the molar ratio of nicotine to alginate monomer of 1:0.8, ethanol as 3 times the mass of alginate, and ethyl acetate as 3 times the mass of nicotine salt;

[0045] Add alginic acid to ethanol and stir to completely swell to obtain alginic acid-ethanol suspension; add nicotine to ethyl acetate and stir to clarify to obtain nicotine ethyl acetate solution; add the obtained nicotine solution dropwise to the obtained alginic acid suspension, stirring and dropping, stirring at room temperature for 3 hours after the dropwise addition is completed to obtain alginic acid-nicotine salt solution, and concentrate under reduced pressure to remove the solvent to obtain a brown-yellow viscous liquid. As for the low-temperature standing and refrigeration in the refrigerator for 3 days, solids precipitate; the obtained solid is crushed and added to ethyl acetate 20 times the mass of alginic acid, stirred for 16 hours, filtered, and the filter cake is washed with ethyl acetate 2-3 times to obtain a brown-yellow solid. The obtained brown-yellow solid is vacuum dried at 65°C to obtain brown-yellow solid nicotine-alginate.

[0046] The total nicotine content of the brown-yellow solid obtained by testing was 46.6%, which was consistent with the theoretical value range of nicotine and alginate salt formation at a molar ratio of 1:1. The yield of solid nicotine-alginate was 81.3%.

[0047] Embodiment 2:

[0048] Prepare the materials according to the molar ratio of nicotine to alginate monomer of 1:0.85, ethanol of 4 times the mass of alginate, and ethyl acetate of 4 times the mass of nicotine salt;

[0049] Add alginic acid to ethanol and stir to completely swell to obtain alginic acid-ethanol suspension; add nicotine to ethyl acetate and stir to clarify to obtain nicotine ethyl acetate solution; add the obtained nicotine solution dropwise to the obtained alginic acid suspension, stirring and dropping, stirring at room temperature for 5 hours after the dropwise addition is completed to obtain alginic acid-nicotine salt solution, and concentrate under reduced pressure to remove the solvent to obtain a brown-yellow viscous liquid. As for the low temperature standing and refrigeration in the refrigerator for 5 days, solids precipitate; the obtained solid is crushed and added to ethyl acetate 30 times the mass of alginic acid, stirred for 16 hours, filtered, and the filter cake is washed with ethyl acetate 2-3 times to obtain a brown-yellow solid. The obtained brown-yellow solid is vacuum dried at 75°C to obtain brown-yellow solid nicotine-alginate.

[0050] The total nicotine content of the brown-yellow solid obtained by testing was 47.1%, which was in line with the theoretical value range of nicotine and alginate salt at a molar ratio of 1:1. The yield of solid nicotine-alginate was 88.3%.

[0051] Embodiment 3:

[0052] The materials were prepared according to the molar ratio of nicotine to alginate monomer of 1:0.95, ethanol of 5 times the mass of alginate, and ethyl acetate of 3 times the mass of nicotine salt;

[0053] Add alginic acid to ethanol and stir to completely swell to obtain alginic acid-ethanol suspension; add nicotine to ethyl acetate and stir to clarify to obtain nicotine ethyl acetate solution; add the obtained nicotine solution dropwise to the obtained alginic acid suspension, stirring and dropping, stirring at room temperature for 4 hours after the dropwise addition is completed to obtain alginic acid-nicotine salt solution, and concentrate under reduced pressure to remove the solvent to obtain a brown-yellow viscous liquid. As for the low temperature standing and refrigeration in the refrigerator for 4 days, solids precipitate; the obtained solid is crushed and added to ethyl acetate 25 times the mass of alginic acid, stirred for 16 hours, filtered, and the filter cake is washed with ethyl acetate 2-3 times to obtain a brown-yellow solid. The obtained brown-yellow solid is vacuum dried at 70°C to obtain brown-yellow solid nicotine-alginate.

[0054] The total nicotine content of the brown-yellow solid obtained by testing was 46.9%, which was consistent with the theoretical value range of nicotine and alginate salt at a molar ratio of 1:1. The yield of solid nicotine-alginate was 90.4.3%.

[0055] Embodiment 4:

[0056] The nicotine-alginate oral cigarette is prepared by mixing the following raw materials in percentage by mass:

[0057] Nicotine-alginate 5%, microcrystalline cellulose 65%, propylene glycol 5%; after mixing and sieving the materials, take the powder with a particle size of 20 mesh and mix them evenly, respectively, and heat them in a pasteurizer, add 10% water, 3% sodium chloride, 2% sodium carbonate, mix them evenly, refrigerate for 12 hours, spray honey 4%, glucose 4%, aspartame 1%, vitamin E1%, seal and refrigerate for 24 hours, sterilize with ultraviolet for 3 hours, and package them into the finished product. The release curve is as follows Figure 2 shown.

[0058] In summary, Examples 1-4 show that the solid nicotine-alginate prepared by the present invention has good properties, is easy to use, has a stable nicotine content, and is suitable for industrial production.

[0059] The present invention relates to the technical field of chemical synthesis, and in particular to a method for preparing nicotine-alginate. The method for preparing nicotine-alginate provided by the present invention uses ethanol and ethyl acetate as reaction solvents and purification solvents; the method is simple and easy to operate, has low production cost, high product salinity, and is suitable for industrialized scale-up production; the obtained solid is a uniform brown-yellow powder, which is applied to new tobacco such as buccal cigarettes and is easy to use.

[0060] The innovative features of the present invention are as follows:

[0061] 1. Use low-toxic ethanol, ethyl acetate and other low-boiling point solvents as reaction solvents for nicotine-alginate synthesis;

[0062] 2. Use low-toxic aprotic low-boiling point solvents such as ethyl acetate as the purification solvent for nicotine-alginate;

[0063] 3. The ratio of nicotine, alginic acid, ethanol and ethyl acetate used, and the temperature used for vacuum drying.

Claims

1. A method for preparing nicotine-alginate for use in buccal cigarettes, characterized in that: Prepared by the following steps: Step 1: Add alginate to a certain amount of ethanol and stir to completely swell it to obtain an alginate-ethanol suspension; Step 2: Add nicotine to a certain amount of ethyl acetate, stir to clarify, and obtain a nicotine ethyl acetate solution; Step 3: Add the ethyl acetate solution of nicotine obtained in step 2 dropwise to the alginate-ethanol suspension obtained in step 1, while stirring. After the addition is complete, stir at room temperature for 3-5 hours to obtain an alginate-nicotine salt solution, and concentrate under reduced pressure to remove the solvent to obtain a brown-yellow viscous liquid, which is placed in a refrigerator and refrigerated for 3-7 days until solids precipitate; Step 4: Crush the solid obtained in step 3, add it to a certain amount of ethyl acetate, stir for 16 hours, filter, wash the filter cake with ethyl acetate 2-3 times to obtain a brown solid, and dry the obtained brown solid in vacuo at 50-75°C to obtain brown solid nicotine-alginate.

2. The method for preparing nicotine-alginate for use in buccal cigarette according to claim 1, characterized in that: The molar ratio of nicotine to alginic acid is 1:0.7-1.

1.

3. The method for preparing nicotine-alginate for use in buccal cigarette according to claim 1, characterized in that: The ethanol added in step 1 is 1-8 times the mass of the alginate.

4. The method for preparing nicotine-alginate for use in buccal cigarette according to claim 1, characterized in that: The amount of ethyl acetate used in step 2 is 1-8 times the mass of nicotine.

5. The method for preparing nicotine-alginate for use in buccal cigarette according to claim 1, characterized in that: In step 4, the mass of ethyl acetate is 10-50 times that of alginate.

6. The method for preparing nicotine-alginate for use in buccal cigarette according to claim 1, characterized in that: In step 4, the ethyl acetate used for washing the filter cake each time is 1-8 times the mass of the alginate.

7. The method for preparing nicotine-alginate for use in buccal cigarette according to claim 1, characterized in that: The vacuum drying temperature is 40-85°C.

8. A nicotine-alginate, characterized in that: Prepared by any one of the methods of claims 1-7.

9. A nicotine-alginate containing buccal cigarette, characterized in that : Prepared by the following method: prepare materials: nicotine-alginate 5%, microcrystalline cellulose 65%, propylene glycol 5%; after mixing and sieving the materials, take powder with a particle size of 20 mesh and mix them evenly, respectively through baking and pasteurization pot heating treatment, add 10% water, 3% sodium chloride, 2% sodium carbonate, mix evenly, refrigerate for 12 hours, spray honey 4%, glucose 4%, aspartame 1%, vitamin E 1%, seal and refrigerate for 24 hours, sterilize by ultraviolet for 3 hours, and package to obtain the finished product; wherein the nicotine-alginate is prepared by any one of claims 1 to 7.

10. A method for preparing a nicotine-alginate oral cigarette, characterized in that: Prepare materials: 5% nicotine-alginate, 65% microcrystalline cellulose, and 5% propylene glycol; after mixing and sieving the materials, take powder particles with a particle size of 20 mesh and mix them evenly, respectively perform baking and heat treatment in a pasteurizer, add 10% water, 3% sodium chloride, and 2% sodium carbonate, mix evenly, refrigerate for 12 hours, spray 4% honey, 4% glucose, 1% aspartame, and 1% vitamin E, seal and refrigerate for 24 hours, sterilize with ultraviolet light for 3 hours, and package to obtain the finished product; wherein the nicotine-alginate is prepared by any one of claims 1 to 7.

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