Fruity wood flavor essence for electronic cigarettes and preparation process thereof

Abstract

This application relates to a fruity wood flavor for electronic cigarettes and its preparation process. The flavor comprises the following components by weight: 10-15 parts antioxidant microcapsules, 15-25 parts grafted chitosan, 3-5 parts surfactant, and 10-20 parts cedar flavor. This application improves the antioxidant, antibacterial, and formaldehyde-scavenging properties of the fruity wood flavor for electronic cigarettes.

Description

Technical Field

[0001] The present application relates to the field of electronic cigarettes, and in particular to a fruit wood flavor essence for electronic cigarettes and a preparation process thereof. Background Art

[0002] E-cigarettes are electronic products that mimic cigarettes. They use high-tech silicon chips and airflow sensors to control smoke output and operating conditions. They atomize a liquid containing extracts, flavors, nicotine, and smoke-generating agents into microparticles that are absorbed by the lungs. E-cigarettes do not contain the tar and other harmful ingredients found in cigarettes, eliminating the risk of secondhand smoke. As a new tobacco product, they offer similar satisfaction to traditional cigarettes while significantly reducing the risk of harm. Therefore, e-cigarettes present a huge market prospect. Flavors are a blend of various spices, resulting in a refreshing aroma. E-cigarette flavors are used to provide a variety of flavors and are typically extracted from nature or synthesized.

[0003] E-cigarette flavors are composed of various aromatic compounds such as esters, alcohols, and phenols. Since some flavors have low boiling points, are volatile, and unstable, they are easily affected by environmental factors when used outdoors. For example, the high temperature, high humidity, and strong ultraviolet rays in summer can promote oxidation or polymerization reactions between aldehydes, alcohols, and unsaturated bond structures and oxygen in the air, so there is room for improvement. Summary of the Invention

[0004] In order to improve the antioxidant properties of fruit wood flavor for electronic cigarettes, the present application provides a fruit wood flavor for electronic cigarettes and a preparation process thereof.

[0005] The present application provides a fruity wood flavor for electronic cigarettes and a preparation process thereof using the following technical solutions:

[0006] In the first aspect, the present application provides a fruit wood flavor for electronic cigarettes, which adopts the following technical solution:

[0007] A fruity wood flavor essence for electronic cigarettes, characterized by comprising the following components in parts by mass:

[0008] 10-15 servings of antioxidant microcapsules

[0009] 15-25 parts grafted chitosan

[0010] 3-5 parts surfactant

[0011] 10-20 parts of cedar flavor essence.

[0012] The cedar flavor provides a fresh and natural aroma that can help refresh the mind and make people energetic; the antioxidant microcapsules enhance the antioxidant properties of the cedar flavor, can help capture and neutralize free radicals, improve the stability of the fruit flavor, and reduce the difficulty of storing the fruit flavor for e-cigarettes; the grafted chitosan wraps the fruit flavor and antioxidant microcapsules through electrostatic interaction to further form a two-layer microcapsule structure, thereby enhancing the antioxidant properties of the fruit flavor, bringing a sustained-release and lasting fragrance effect to the fruit flavor for e-cigarettes, and enhancing the user experience.

[0013] Preferably, the antioxidant microcapsules include sodium alginate, a grafted tripeptide and a cross-linking agent.

[0014] Sodium alginate has good antioxidant properties, antibacterial properties, biocompatibility, non-toxicity and biodegradability. Its aqueous solution has a high viscosity and can coat and protect the grafted tripeptide to achieve a long-lasting antioxidant effect. The grafted tripeptide has good stability and compatibility through the combination design of three amino acids and grafting modification. By using sodium alginate to coat the grafted tripeptide, a sustained release effect can be achieved, realizing long-lasting antioxidant properties. The cross-linker promotes the coating of the grafted polypeptide with sodium alginate by adjusting the positive charge of the grafted polypeptide.

[0015] Preferably, the grafted tripeptide comprises methyl methacrylate functionalized dextran and His-Lys-Cys tripeptide (histidine-lysine-cysteine ​​tripeptide).

[0016] Glucan has the effects of improving immunity, antiviral and reducing sensitivity. By functionalizing glucan with methyl methacrylate, the double bonds of glucan and His-Lys-Cys tripeptide can undergo addition reaction; methyl methacrylate functionalized glucan can also improve the dispersibility and stability of the tripeptide and reduce the aggregation between the tripeptides; His-Lys-Cys tripeptide is designed from a combination of histidine, lysine and cysteine. These three amino acids can capture and neutralize free radicals and have good antioxidant capacity. Cysteine ​​and lysine have good antibacterial properties. The synthesized His-Lys-Cys tripeptide can combine with bacterial biofilms to form pores, causing the leakage of bacterial cell contents, thereby causing bacterial apoptosis; the three amino acids have good reactivity with aldehydes. The amino groups on the three amino acids can undergo condensation reaction with formaldehyde to achieve the effect of removing formaldehyde, reducing the impact of formaldehyde generated during the atomization process of electronic cigarettes on the human body and improving the safety performance of electronic cigarettes.

[0017] Preferably, the mass ratio of the sodium alginate, the grafted tripeptide and the cross-linking agent is 1:(0.5-0.8):0.05.

[0018] The fruity wood flavor essence for electronic cigarettes obtained according to the above mass ratio has good antioxidant and antibacterial properties.

[0019] Preferably, the cross-linking agent is tannic acid.

[0020] Tannic acid is composed of repeating units such as glucose and gallic acid. It can be used as a cross-linking agent to increase the positive charge of the solution and promote the reaction of sodium alginate coated with the grafted tripeptide. Tannic acid can also serve as a bridge connecting sodium alginate and chitosan. Hydrogen bonds are formed between tannic acid and grafted chitosan, promoting the rapid cross-linking of grafted chitosan with antioxidant microcapsules. Tannic acid contains a large number of hydroxyl groups in its structure and has good antioxidant properties. It can effectively remove various free radicals and destroy bacterial cell membranes. Using tannic acid as a cross-linking agent can synergistically improve the antioxidant and antibacterial properties of antioxidant microcapsules with sodium alginate and grafted tripeptide.

[0021] Preferably, the antioxidant microcapsules are prepared by the following steps:

[0022] dissolving dextran, sodium hydroxide, and glycidyl methacrylate in anhydrous ethanol to obtain a reaction solution, neutralizing excess sodium hydroxide with hydrochloric acid after the reaction, dialyzing and freeze-drying the resulting solution to obtain methyl methacrylate-functionalized dextran;

[0023] Dissolving His-Lys-Cys tripeptide, methyl methacrylate functionalized dextran and sodium hydroxide in phosphate buffer to obtain a mixed solution, vortexing the mixed solution, neutralizing excess sodium hydroxide with hydrochloric acid, desalting and purifying, and then freeze-drying to obtain a grafted tripeptide;

[0024] The grafted tripeptide is dissolved in phosphate buffer to obtain a grafted tripeptide solution, sodium alginate and tannic acid are dissolved in deionized water to obtain a sodium alginate solution, the sodium alginate solution, Tween-80 and calcium chloride are added to the grafted tripeptide solution under stirring conditions to react, and the resulting solution is centrifuged and washed to obtain antioxidant microcapsules.

[0025] The antioxidant microcapsules prepared according to the above steps have good antioxidant properties, antibacterial properties and formaldehyde scavenging capabilities.

[0026] Preferably, the grafted chitosan comprises chitosan, chlorogenic acid amide and a coupling agent.

[0027] Chlorogenic acid amide is formed by the condensation of chlorogenic acid and nicotinamide. Chlorogenic acid contains a large number of hydroxyl groups, which can form hydrogen free radicals with antioxidant effects to eliminate the activity of free radicals such as hydroxyl free radicals and superoxide anions, and has antibacterial, anti-inflammatory, antioxidant and free radical scavenging effects; nicotinamide is a derivative of nicotinic acid, which can help scavenge free radicals and has good antioxidant properties. Chlorogenic acid amide obtained by dimerization of nicotinamide and chlorogenic acid has good stability; chlorogenic acid amide can also enhance the positive charge of grafted chitosan, increase the cross-linking of grafted chitosan and antioxidant microcapsules, and enhance the stability of fruity wood flavor for electronic cigarettes, thereby enhancing the antioxidant properties of fruity wood flavor for electronic cigarettes; chlorogenic acid amide and antioxidant microcapsules can also synergistically enhance the antioxidant and antibacterial properties of grafted chitosan, while preventing and treating the occurrence of inflammation, thereby enhancing the safety performance of fruity wood flavor for electronic cigarettes.

[0028] Preferably, the mass ratio of the chitosan, chlorogenic acid amide and coupling agent is 1:(0.05-0.15):0.05.

[0029] The fruity wood flavor essence for electronic cigarettes obtained according to the above mass ratio has good antioxidant and antibacterial properties.

[0030] Preferably, the coupling agent is N-hydroxysuccinimide.

[0031] N-hydroxysuccinimide can be used as a coupling agent to improve the efficiency of chlorogenic acid amide grafting chitosan; N-hydroxysuccinimide can react with the amino group of the grafted tripeptide to promote the cross-linking of antioxidant microcapsules and grafted chitosan; N-hydroxysuccinimide also has the effect of lightening spots, can complex with highly oxidizing substances, reduce the impact of highly oxidizing substances on oral health, and synergize with chlorogenic acid amide and antioxidant microcapsules to enhance the antioxidant properties of fruity wood flavors for e-cigarettes.

[0032] In a second aspect, the present application provides a preparation process for a fruity wood flavor for electronic cigarettes, which adopts the following technical solution:

[0033] A fruity wood flavor essence for electronic cigarettes is prepared by the following steps:

[0034] dispersing cedar flavor essence and surfactant in deionized water to obtain emulsified flavor essence;

[0035] dispersing antioxidant microcapsules and Tween-80 into emulsified flavor to obtain a dispersion;

[0036] The grafted chitosan is added to the dispersion under stirring conditions, the pH is adjusted and then centrifuged to obtain a product, and the product is washed and dried to obtain a fruity wood flavor essence for electronic cigarettes.

[0037] The fruity wood flavor essence for electronic cigarettes prepared according to the above steps has good antioxidant and antibacterial properties.

[0038] In summary, this application includes at least one of the following beneficial technical effects:

[0039] 1. Antioxidant microcapsules enhance the antioxidant properties of cedar flavor, can help capture and neutralize free radicals, improve the stability of fruity flavor, and reduce the difficulty of storing fruity flavor for e-cigarettes; grafted chitosan wraps the fruity flavor and antioxidant microcapsules through electrostatic interaction to further form a two-layer microcapsule structure, thereby enhancing the antioxidant properties of the fruity flavor, bringing a sustained-release and lasting fragrance effect to the fruity flavor for e-cigarettes, and improving the user experience.

[0040] 2. Grafted tripeptide and chlorogenic acid amide have good antioxidant and antibacterial properties. The synergistic effect of the two can prevent and treat the occurrence of inflammation, help quench the generated free radicals, relieve stress response, reduce the probability of oral problems, and improve the safety of fruity wood flavors for e-cigarettes.

[0041] 3. The two-layer sac structure protects the grafted tripeptide and cedar flavor, making the fruity flavor for electronic cigarettes have a sustained-release and lasting fragrance effect. The grafted tripeptide protected by the two-layer sac structure can exert long-lasting antioxidant and antibacterial properties. DETAILED DESCRIPTION

[0042] The present application discloses a fruit wood flavor essence for electronic cigarettes and a preparation process thereof. The present application is further described in detail below with reference to the examples:

[0043] Example

[0044] Example 1

[0045] Preparation of antioxidant microcapsules

[0046] 15.0 g of dextran (CAS No. 9004-54-0) was dissolved in 100 mL of anhydrous ethanol and magnetically stirred until fully dissolved. 1 g of sodium hydroxide was added and nitrogen was introduced for 20 minutes to expel air from the system. Then, 4 mL of glycidyl methacrylate (CAS No. 106-91-2) was added to the system to obtain a reaction solution. The reaction solution was magnetically stirred for 8 hours at room temperature in the dark. The excess sodium hydroxide in the reaction solution was neutralized with hydrochloric acid. The neutralized reaction solution was placed in a dialysis bag with a cutoff of 3500 Da and dialyzed against deionized water in the dark with an ice bath for 8 hours. The dialyzed reaction solution was frozen and lyophilized in a freeze dryer to obtain methyl methacrylate-functionalized dextran.

[0047] 0.2 g of His-Lys-Cys tripeptide (synthesized by Hangzhou Zhuanpeptide Biotechnology Co., Ltd.), 11 g of methyl methacrylate-functionalized dextran, and 1.1 g of sodium hydroxide were dissolved in 50 mL of phosphate buffer and sonicated to obtain a mixed solution. The mixed solution was vortexed for 8 h to obtain a reacted mixed solution. The excess sodium hydroxide was neutralized with hydrochloric acid. The neutralized solution was desalted and purified using a Zeba desalting centrifugal column (7K MWCO) and then freeze-dried to obtain the grafted tripeptide.

[0048] 6.5 g of the grafted tripeptide was dissolved in 50 mL of phosphate buffer to obtain a grafted tripeptide solution, 13 g of sodium alginate (CAS number: 9005-38-3) and 0.65 g of tannic acid (CAS number: 1401-55-4) were dissolved in 50 mL of deionized water to obtain a sodium alginate solution, and the sodium alginate solution, 1 g of Tween-80 and 2 g of calcium chloride were added to the grafted tripeptide solution under stirring conditions. After reacting for 10 minutes, the mixture was centrifuged and washed with deionized water to obtain antioxidant microcapsules.

[0049] Preparation of grafted chitosan

[0050] Combine 20g of chlorogenic acid (CAS No. 1401-55-4) and 6.9g of nicotinamide (CAS No. 98-92-0) in a 500mL round-bottom flask. Under fluorine gas, add 140mL of anhydrous ethanol and stir until dissolved. Add 2.0g of N,N-diisopropylethylamine (CAS No. 7087-68-5) and 0.22g of ethylenediamine (CAS No. 107-15-3) to the round-bottom flask. After reacting for 6 hours, evaporate the solvent under reduced pressure to obtain a crude product. Purify the crude product by silica gel column chromatography, eluting with dichloromethane-methanol in a volume ratio of 20:1, and drying to obtain chlorogenic acid amide.

[0051] 1.4 g of chlorogenic acid amide was dispersed in 40 mL of anhydrous ethanol, 1.4 g of N-hydroxysuccinimide (CAS number: 6066-82-6) was added to the anhydrous ethanol, and the mixture was stirred to obtain a grafting solution; 27.3 g of chitosan (CAS number: 9012-76-4) was dissolved in 600 g of 2.5% acetic acid solution, and stirred with a magnetic stirrer until completely dissolved to obtain a chitosan solution; the grafting solution was added dropwise to the chitosan solution at a rate of 30 drops / min, and the mixture was reacted in a 60 ° C water bath for 2 h. After the reaction was completed, the reaction solution was cooled to room temperature, and the reaction solution was poured into 500 mL of anhydrous ethanol for precipitation and filtered to obtain a crude product. The crude product was redissolved with 2.5% acetic acid solution, and then precipitated with anhydrous ethanol to obtain a precipitate. The precipitate was washed three times with anhydrous ethanol, and finally the washed precipitate was dried in a vacuum freeze dryer at -20 ° C to constant weight to obtain grafted chitosan.

[0052] Preparation of fruity wood flavor for electronic cigarettes

[0053] 10 g of benzyl benzoate, 3.5 g of methyl cedar ketone, 3 g of Atlantic cedar essential oil, 2.5 g of galaxol, 2 g of terpineol acetate, 2 g of sandalwood, 2 g of synthetic linalool, 1.5 g of pine needle oil, 1.5 g of Brazilian sweet orange oil, 1 g of linalyl acetate, 0.5 g of terpineol methyl, 0.5 g of crystalline cedarol, 0.2 g of patchouli oil, 0.05 g of vanillin, 0.05 g of borneol and 0.02 g of ethyl maltol were mixed and stirred to obtain a cedar flavor essence.

[0054] Disperse 10 g of cedar flavor and 3 g of hydrogenated soybean lecithin (CAS No.: 92128-87-5) in deionized water to obtain an emulsified flavor;

[0055] Dispersing 10 g of antioxidant microcapsules and 1 g of Tween-80 into the emulsified flavor to obtain a dispersion;

[0056] Under stirring conditions, 15 g of grafted chitosan was dissolved in 300 g of acetic acid solution with a mass fraction of 2.5% to obtain a grafted chitosan solution. The grafted chitosan solution was added to the dispersion, and the pH was adjusted to 3.0 with hydrochloric acid. After reacting for 15 minutes, the product was centrifuged to obtain the product. The product was washed three times with deionized water and dried in an oven at 40°C to obtain a fruity wood flavor for electronic cigarettes.

[0057] Example 2

[0058] Preparation of antioxidant microcapsules

[0059] 15.0 g of dextran (CAS No. 9004-54-0) was dissolved in 100 mL of anhydrous ethanol and magnetically stirred until fully dissolved. 1 g of sodium hydroxide was added and nitrogen was introduced for 20 minutes to expel air from the system. Then, 4 mL of glycidyl methacrylate (CAS No. 106-91-2) was added to the system to obtain a reaction solution. The reaction solution was magnetically stirred for 8 hours at room temperature in the dark. The excess sodium hydroxide in the reaction solution was neutralized with hydrochloric acid. The neutralized reaction solution was placed in a dialysis bag with a cutoff of 3500 Da and dialyzed against deionized water in the dark with an ice bath for 8 hours. The dialyzed reaction solution was frozen and lyophilized in a freeze dryer to obtain methyl methacrylate-functionalized dextran.

[0060] 0.2 g of His-Lys-Cys tripeptide (synthesized by Hangzhou Zhuanpeptide Biotechnology Co., Ltd.), 11 g of methyl methacrylate-functionalized dextran, and 1.1 g of sodium hydroxide were dissolved in 50 mL of phosphate buffer and sonicated to obtain a mixed solution. The mixed solution was vortexed for 8 h to obtain a reacted mixed solution. The excess sodium hydroxide was neutralized with hydrochloric acid. The neutralized solution was desalted and purified using a Zeba desalting centrifugal column (7K MWCO) and then freeze-dried to obtain the grafted tripeptide.

[0061] 8.65 g of the grafted tripeptide was dissolved in 50 mL of phosphate buffer to obtain a grafted tripeptide solution, 10.85 g of sodium alginate (CAS number: 9005-38-3) and 0.55 g of tannic acid (CAS number: 1401-55-4) were dissolved in 50 mL of deionized water to obtain a sodium alginate solution, and the sodium alginate solution, 1 g of Tween-80 and 2 g of calcium chloride were added to the grafted tripeptide solution under stirring conditions. After reacting for 10 minutes, the mixture was centrifuged and washed with deionized water to obtain antioxidant microcapsules.

[0062] Preparation of grafted chitosan

[0063] Combine 20g of chlorogenic acid (CAS No. 1401-55-4) and 6.9g of nicotinamide (CAS No. 98-92-0) in a 500mL round-bottom flask. Under fluorine gas, add 140mL of anhydrous ethanol and stir until dissolved. Add 2.0g of N,N-diisopropylethylamine (CAS No. 7087-68-5) and 0.22g of ethylenediamine (CAS No. 107-15-3) to the round-bottom flask. After reacting for 6 hours, evaporate the solvent under reduced pressure to obtain a crude product. Purify the crude product by silica gel column chromatography, eluting with dichloromethane-methanol in a volume ratio of 20:1, and drying to obtain chlorogenic acid amide.

[0064] 3.8 g of chlorogenic acid amide was dispersed in 40 mL of anhydrous ethanol, 1.3 g of N-hydroxysuccinimide (CAS number: 6066-82-6) was added to the anhydrous ethanol, and the mixture was stirred to obtain a grafting solution; 25.1 g of chitosan (CAS number: 9012-76-4) was dissolved in 600 g of 2.5% acetic acid solution, and stirred with a magnetic stirrer until completely dissolved to obtain a chitosan solution; the grafting solution was added dropwise to the chitosan solution at a rate of 30 drops / min, and the mixture was reacted in a 60 ° C water bath for 2 h. After the reaction was completed, the reaction solution was cooled to room temperature, and the reaction solution was poured into 500 mL of anhydrous ethanol for precipitation and filtered to obtain a crude product. The crude product was redissolved with 2.5% acetic acid solution, and then precipitated with anhydrous ethanol to obtain a precipitate. The precipitate was washed three times with anhydrous ethanol, and finally the washed precipitate was dried in a vacuum freeze dryer at -20 ° C to constant weight to obtain grafted chitosan.

[0065] Preparation of fruity wood flavor for electronic cigarettes

[0066] 10 g of benzyl benzoate, 3.5 g of methyl cedar ketone, 3 g of Atlantic cedar essential oil, 2.5 g of galaxol, 2 g of terpineol acetate, 2 g of sandalwood, 2 g of synthetic linalool, 1.5 g of pine needle oil, 1.5 g of Brazilian sweet orange oil, 1 g of linalyl acetate, 0.5 g of terpineol methyl, 0.5 g of crystalline cedarol, 0.2 g of patchouli oil, 0.05 g of vanillin, 0.05 g of borneol and 0.02 g of ethyl maltol were mixed and stirred to obtain a cedar flavor essence.

[0067] Disperse 20 g of cedar flavor and 5 g of hydrogenated soybean lecithin (CAS No.: 92128-87-5) in deionized water to obtain an emulsified flavor;

[0068] Dispersing 15 g of antioxidant microcapsules and 1.5 g of Tween-80 into the emulsified flavor to obtain a dispersion;

[0069] Under stirring conditions, 25 g of grafted chitosan was dissolved in 300 g of acetic acid solution with a mass fraction of 2.5% to obtain a grafted chitosan solution. The grafted chitosan solution was added to the dispersion, and the pH was adjusted to 3.0 with hydrochloric acid. After reacting for 15 minutes, the product was centrifuged to obtain the product. The product was washed three times with deionized water and dried in an oven at 40°C to obtain a fruity wood flavor for electronic cigarettes.

[0070] Example 3

[0071] Preparation of antioxidant microcapsules

[0072] 15.0 g of dextran (CAS No. 9004-54-0) was dissolved in 100 mL of anhydrous ethanol and magnetically stirred until fully dissolved. 1 g of sodium hydroxide was added and nitrogen was introduced for 20 minutes to expel air from the system. Then, 4 mL of glycidyl methacrylate (CAS No. 106-91-2) was added to the system to obtain a reaction solution. The reaction solution was magnetically stirred for 8 hours at room temperature in the dark. The excess sodium hydroxide in the reaction solution was neutralized with hydrochloric acid. The neutralized reaction solution was placed in a dialysis bag with a cutoff of 3500 Da and dialyzed against deionized water in the dark with an ice bath for 8 hours. The dialyzed reaction solution was frozen and lyophilized in a freeze dryer to obtain methyl methacrylate-functionalized dextran.

[0073] 0.2 g of His-Lys-Cys tripeptide (synthesized by Hangzhou Zhuanpeptide Biotechnology Co., Ltd.), 11 g of methyl methacrylate-functionalized dextran, and 1.1 g of sodium hydroxide were dissolved in 50 mL of phosphate buffer and sonicated to obtain a mixed solution. The mixed solution was vortexed for 8 h to obtain a reacted mixed solution. The excess sodium hydroxide was neutralized with hydrochloric acid. The neutralized solution was desalted and purified using a Zeba desalting centrifugal column (7K MWCO) and then freeze-dried to obtain the grafted tripeptide.

[0074] 7.65 g of the grafted tripeptide was dissolved in 50 mL of phosphate buffer to obtain a grafted tripeptide solution, 11.8 g of sodium alginate (CAS number: 9005-38-3) and 0.6 g of tannic acid (CAS number: 1401-55-4) were dissolved in 50 mL of deionized water to obtain a sodium alginate solution, and the sodium alginate solution, 1 g of Tween-80 and 2 g of calcium chloride were added to the grafted tripeptide solution under stirring conditions. After reacting for 10 minutes, the mixture was centrifuged and washed with deionized water to obtain antioxidant microcapsules.

[0075] Preparation of grafted chitosan

[0076] Combine 20g of chlorogenic acid (CAS No. 1401-55-4) and 6.9g of nicotinamide (CAS No. 98-92-0) in a 500mL round-bottom flask. Under fluorine gas, add 140mL of anhydrous ethanol and stir until dissolved. Add 2.0g of N,N-diisopropylethylamine (CAS No. 7087-68-5) and 0.22g of ethylenediamine (CAS No. 107-15-3) to the round-bottom flask. After reacting for 6 hours, evaporate the solvent under reduced pressure to obtain a crude product. Purify the crude product by silica gel column chromatography, eluting with dichloromethane-methanol in a volume ratio of 20:1, and drying to obtain chlorogenic acid amide.

[0077] 2.65 g of chlorogenic acid amide was dispersed in 40 mL of anhydrous ethanol, 1.35 g of N-hydroxysuccinimide (CAS number: 6066-82-6) was added to the anhydrous ethanol, and the mixture was stirred to obtain a grafting solution; 26.1 g of chitosan (CAS number: 9012-76-4) was dissolved in 600 g of 2.5% acetic acid solution, and stirred with a magnetic stirrer until completely dissolved to obtain a chitosan solution; the grafting solution was added dropwise to the chitosan solution at a rate of 30 drops / min, and the mixture was reacted in a 60 ° C water bath for 2 h. After the reaction was completed, the reaction solution was cooled to room temperature, and the reaction solution was poured into 500 mL of anhydrous ethanol for precipitation and filtered to obtain a crude product. The crude product was redissolved with 2.5% acetic acid solution, and then precipitated with anhydrous ethanol to obtain a precipitate. The precipitate was washed three times with anhydrous ethanol, and finally the washed precipitate was dried in a vacuum freeze dryer at -20 ° C to constant weight to obtain grafted chitosan.

[0078] Preparation of fruity wood flavor for electronic cigarettes

[0079] 10 g of benzyl benzoate, 3.5 g of methyl cedar ketone, 3 g of Atlantic cedar essential oil, 2.5 g of galaxol, 2 g of terpineol acetate, 2 g of sandalwood, 2 g of synthetic linalool, 1.5 g of pine needle oil, 1.5 g of Brazilian sweet orange oil, 1 g of linalyl acetate, 0.5 g of terpineol methyl, 0.5 g of crystalline cedarol, 0.2 g of patchouli oil, 0.05 g of vanillin, 0.05 g of borneol and 0.02 g of ethyl maltol were mixed and stirred to obtain a cedar flavor essence.

[0080] Disperse 15 g of cedar flavor and 4 g of hydrogenated soybean lecithin (CAS No.: 92128-87-5) in deionized water to obtain an emulsified flavor;

[0081] Dispersing 12.5 g of antioxidant microcapsules and 1.25 g of Tween-80 into the emulsified flavor to obtain a dispersion;

[0082] Under stirring conditions, 25 g of grafted chitosan was dissolved in 300 g of acetic acid solution with a mass fraction of 2.5% to obtain a grafted chitosan solution. The grafted chitosan solution was added to the dispersion, and the pH was adjusted to 3.0 with hydrochloric acid. After reacting for 15 minutes, the product was centrifuged to obtain the product. The product was washed three times with deionized water and dried in an oven at 40°C to obtain a fruity wood flavor for electronic cigarettes.

[0083] Example 4

[0084] Example 4 is based on Example 3. The only difference between Example 4 and Example 3 is that in Example 4, the amount of sodium alginate used is 14.85 g, the amount of grafted tripeptide used is 4.45 g, and the amount of tannic acid used is 0.75 g.

[0085] Example 5

[0086] Example 5 is based on Example 3. The only difference between Example 5 and Example 3 is that in Example 5, the amount of sodium alginate used is 9.8 g, the amount of grafted tripeptide used is 9.8 g, and the amount of tannic acid used is 0.5 g.

[0087] Example 6

[0088] Example 6 is based on Example 3. The only difference between Example 6 and Example 3 is that in Example 6, the amount of chitosan used is 28.1 g, the amount of chlorogenic acid amide used is 0.6 g, and the amount of coupling agent used is 1.45 g.

[0089] Example 7

[0090] Example 7 is based on Example 3. The only difference between Example 7 and Example 3 is that in Example 7, the amount of chitosan used is 24.1 g, the amount of chlorogenic acid amide used is 4.85 g, and the amount of coupling agent used is 1.2 g.

[0091] Comparative Example 1

[0092] Comparative Example 1 is based on Example 3. The only difference between Comparative Example 1 and Example 3 is that in Comparative Example 1, no grafted tripeptide is added during the step of preparing the antioxidant microcapsules.

[0093] Comparative Example 2

[0094] Comparative Example 2 is based on Example 3. The only difference between Comparative Example 2 and Example 3 is that in Comparative Example 2, the grafted tripeptide is replaced by a His-Lys-Cys tripeptide.

[0095] Comparative Example 3

[0096] Comparative Example 3 is based on Example 3, and the only difference between Comparative Example 3 and Example 3 is that chlorogenic acid amide is replaced by chlorogenic acid in Comparative Example 3.

[0097] Comparative Example 4

[0098] Comparative Example 4 is based on Example 3, and the only difference between Comparative Example 4 and Example 3 is that chlorogenic acid amide is replaced by nicotinic acid in Comparative Example 4.

[0099] Comparative Example 5

[0100] Comparative Example 5 is based on Example 3. The only difference between Comparative Example 5 and Example 3 is that tannic acid is not added in the step of preparing the antioxidant microcapsules in Comparative Example 5.

[0101] Comparative Example 6 is based on Example 3. The only difference between Comparative Example 6 and Example 3 is that in Comparative Example 6, N-hydroxysuccinimide is replaced by N,N'-methylenebisacrylamide.

[0102] Performance testing

[0103] (1) Determination of the antioxidant properties of fruity wood flavor for electronic cigarettes: 0.2 mmol / L DPPH was prepared with 95% ethanol, and the fruity wood flavor for electronic cigarettes was prepared into a 1 mg / mL dispersion. 100uL of the dispersion was mixed with 100uL of DPPH solution in a 96-well ELISA plate, and the mixture was reacted at room temperature in the dark for 30 minutes. The absorbance value A1 was measured at 517nm. 100uL of 95% ethanol was used instead of DPPH solution to react with 100uL deionized water as the blank control group (A0), and 100uL of DPPH solution was used to react with 100uL deionized water as the negative control group (A2). The DPPH clearance rate was calculated as follows: DPPH clearance rate (%) = (A2-A1) / (A2-A0)*100%. Each sample was tested three times, and the average value was taken after measurement. The results are recorded in Table 1.

[0104] (2) Determination of the antibacterial properties of fruity wood flavor for electronic cigarettes: The fruity wood flavor for electronic cigarettes was prepared into a dispersion with a concentration of 1 mg / mL using distilled water. The sample was placed in a sterilized culture dish, and the bacterial solution containing Escherichia coli was added dropwise to the sample and mixed evenly. The sample was cultured at a constant temperature for 24 hours under the same conditions, and the sterilization rate of each sample was then determined. Each sample was tested three times, and the average value was calculated after the test. The results are recorded in Table 1.

[0105] (3) Determination of the formaldehyde removal ability of fruit wood flavor for electronic cigarettes: The fruit wood flavor for electronic cigarettes was prepared into a dispersion with a concentration of 1 mg / mL using distilled water. The dispersion was mixed with a 1 mg / mL formaldehyde solution. After standing for 30 minutes, the formaldehyde concentration in the solution was measured and the formaldehyde removal rate was calculated. Each sample was tested three times, and the average value was taken after measurement. The results are recorded in Table 1.

[0106] Table 1 Test results of antioxidant, antibacterial and formaldehyde removal performance of fruit wood flavor for electronic cigarettes

[0107] Test results DPPH clearance rate / % Escherichia coli sterilization rate / % Formaldehyde removal rate / % Example 1 98.5 98.8 97.3 Example 2 98.8 99.1 98.2 Example 3 99.3 99.5 98.7 Example 4 95.2 94.3 93.3 Example 5 96.1 95.2 93.6 Example 6 93.3 93.7 97.1 Example 7 94.5 94.0 96.9 Comparative Example 1 50.3 46.9 22.1 Comparative Example 2 76.5 79.1 69.3 Comparative Example 3 79.2 78.9 90.5 Comparative Example 4 77.9 78.4 89.8 Comparative Example 5 69.7 71.2 88.2 Comparative Example 6 82.3 85.1 88.4

[0108] As can be seen from Table 1, the DPPH removal rates of Examples 1-3 are all above 98.5%, the E. coli sterilization rates are all above 98.8%, and the formaldehyde removal rates are all above 97.3%. It can be seen that the fruity wood flavor for electronic cigarettes prepared in this application has good antioxidant properties, antibacterial properties and formaldehyde removal capabilities.

[0109] As can be seen from Table 1, the only difference between Example 4 and Example 3 is that the mass ratio in Example 4 is 1:0.3:0.05, and the mass ratio in Example 3 is 1:0.65:0.05. The DPPH removal rate in Example 4 is 95.2%, the Escherichia coli sterilization rate is 94.3%, and the formaldehyde removal rate is 93.3%. The DPPH removal rate in Example 3 is 99.3%, the Escherichia coli sterilization rate is 99.5%, and the formaldehyde removal rate is 98.7%. Compared with Example 3, the antioxidant performance, antibacterial performance and formaldehyde removal ability of Example 4 are all reduced; this is because the amount of sodium alginate and tannic acid is increased and the amount of grafted tripeptide is reduced, resulting in a weakening of the synergistic effect of the antioxidant microcapsules and chlorogenic acid amide, thereby reducing the antioxidant and antibacterial properties of the fruity wood flavor for electronic cigarettes; the reduced content of the grafted tripeptide in the antioxidant microcapsules leads to a reduction in the reactive sites for formaldehyde, and the formaldehyde removal ability is reduced.

[0110] As can be seen from Table 1, the only difference between Example 5 and Example 3 is that the mass ratio in Example 5 is 1:1:0.05, the DPPH removal rate in Example 5 is 96.1%, the Escherichia coli sterilization rate is 95.2%, and the formaldehyde removal rate is 93.6%. Compared with Example 3, the antioxidant performance, antibacterial performance and formaldehyde removal ability of Example 5 are all reduced; this is because the amount of grafted tripeptide is increased, the amount of sodium alginate and tannic acid is reduced, the sodium alginate cannot fully embed the grafted tripeptide, the cross-linking degree of the antioxidant microcapsules and the grafted chitosan is reduced, and the stability of the fruity wood flavor for electronic cigarettes is reduced, thereby reducing the antioxidant performance, antibacterial performance and formaldehyde removal ability.

[0111] As can be seen from Table 1, the only difference between Example 6 and Example 3 is that the mass ratio in Example 6 is 1:0.02:0.05, and the mass ratio in Example 3 is 1:0.2:0.05. The DPPH removal rate in Example 6 is 93.3%, the Escherichia coli sterilization rate is 93.7%, and the formaldehyde removal rate is 97.1%. Compared with Example 3, Example 6 has reduced antioxidant performance, antibacterial performance and formaldehyde removal ability; this is because the amount of chlorogenic acid amide is reduced, the amount of chitosan and coupling agent is increased, the synergistic effect between chlorogenic acid amide and antioxidant microcapsules is weakened, and the number of free radicals that can be captured and quenched by grafted chitosan is reduced. Therefore, the antioxidant performance, antibacterial performance and formaldehyde removal ability of the fruity wood flavor for electronic cigarettes are reduced.

[0112] As can be seen from Table 1, the only difference between Example 7 and Example 3 is that the mass ratio in Example 7 is 1:0.2:0.05, the DPPH removal rate in Example 7 is 94.5%, the Escherichia coli sterilization rate is 94.0%, and the formaldehyde removal rate is 96.9%. Compared with Example 3, the antioxidant performance, antibacterial performance and formaldehyde removal ability of Example 7 are all reduced; this is because the amount of chlorogenic acid amide is increased, the amount of chitosan and coupling agent is reduced, and the stability of the grafted chitosan is reduced, so that the overall stability of the fruity wood flavor for electronic cigarettes is reduced, and the antioxidant performance, antibacterial performance and formaldehyde removal ability are all reduced.

[0113] As can be seen from Table 1, the only difference between Comparative Example 1 and Example 3 is that in Comparative Example 1, no grafted tripeptide is added in the step of preparing the antioxidant microcapsules. The DPPH scavenging rate in Comparative Example 1 is 50.3%, the Escherichia coli sterilization rate is 46.9%, and the formaldehyde scavenging rate is 22.1%. Compared with Example 3, Comparative Example 1 has significantly decreased antioxidant performance, antibacterial performance, and formaldehyde scavenging ability. This is because without the addition of the grafted tripeptide, the ability of the antioxidant microcapsules to scavenge free radicals is weakened, the sites for quenching bacteria are reduced, and the reaction sites for formaldehyde are reduced. At the same time, the synergistic effect of the antioxidant microcapsules and chlorogenic acid amide is weakened, so the antioxidant performance, antibacterial performance, and formaldehyde scavenging ability are all reduced.

[0114] As can be seen from Table 1, the only difference between Comparative Example 2 and Example 3 is that the grafted tripeptide is replaced by His-Lys-Cys tripeptide in Comparative Example 2. The DPPH removal rate in Comparative Example 2 is 76.5%, the Escherichia coli sterilization rate is 79.1%, and the formaldehyde removal rate is 69.3%. Compared with Example 3, Comparative Example 2 has significantly reduced antioxidant performance, antibacterial performance, and formaldehyde removal ability. This is because the grafted tripeptide is replaced by His-Lys-Cys tripeptide, and the His-Lys-Cys tripeptide lacks the grafting modification of methyl methacrylate functionalized dextran. The stability of the His-Lys-Cys tripeptide is reduced, and the overall stability of the fruity wood flavor for electronic cigarettes is reduced, thereby reducing the antioxidant performance, antibacterial performance, and formaldehyde removal ability.

[0115] As can be seen from Table 1, the only difference between Comparative Example 3 and Example 3 is that chlorogenic acid amide is replaced by chlorogenic acid in Comparative Example 3. The DPPH removal rate in Comparative Example 3 is 79.2%, the Escherichia coli sterilization rate is 78.9%, and the formaldehyde removal rate is 90.5%. Compared with Example 3, the antioxidant performance, antibacterial performance and formaldehyde removal ability of Comparative Example 3 are greatly reduced; this is because chlorogenic acid amide is replaced by chlorogenic acid, the stability of chlorogenic acid is poor, and there is a lack of synergistic effect with nicotinamide, and the antioxidant performance, antibacterial performance and stability of the grafted chitosan are reduced; the synergistic effect of chlorogenic acid and antioxidant microcapsules is weakened, so that the antioxidant performance, antibacterial performance and formaldehyde removal ability of the fruity wood flavor for electronic cigarettes are reduced.

[0116] As can be seen from Table 1, the only difference between Comparative Example 4 and Example 3 is that chlorogenic acid amide is replaced by nicotinic acid in Comparative Example 4. The DPPH removal rate in Comparative Example 4 is 77.9%, the E. coli sterilization rate is 78.4%, and the formaldehyde removal rate is 89.8%. Compared with Example 3, the antioxidant performance, antibacterial performance and formaldehyde removal ability of Comparative Example 4 are all reduced; this is because chlorogenic acid amide is replaced by nicotinic acid, and nicotinic acid can react to obtain nicotinamide, but nicotinic acid alone lacks the synergistic effect with chlorogenic acid. At the same time, the synergistic effect of nicotinic acid and antioxidant microcapsules is weakened. Therefore, the antioxidant performance, antibacterial performance and formaldehyde removal ability of the fruity wood flavor for electronic cigarettes are all reduced.

[0117] As can be seen from Table 1, the only difference between Comparative Example 5 and Example 3 is that tannic acid is not added in the step of preparing the antioxidant microcapsules in Comparative Example 5. The DPPH removal rate in Comparative Example 5 is 69.7%, the Escherichia coli sterilization rate is 71.2%, and the formaldehyde removal rate is 88.2%. Compared with Example 3, the antioxidant performance, antibacterial performance and formaldehyde removal ability of Comparative Example 5 are all reduced; this is because tannic acid is not added in the step of preparing the antioxidant microcapsules, and there is a lack of tannic acid as a cross-linking agent. The embedding effect of sodium alginate on the grafted tripeptide is reduced, the cross-linking between the antioxidant microcapsules and the grafted chitosan is reduced, and the overall stability of the fruity wood flavor for electronic cigarettes is reduced. Therefore, the antioxidant performance, antibacterial performance and formaldehyde removal ability of the fruity wood flavor for electronic cigarettes are all reduced.

[0118] As can be seen from Table 1, the only difference between Comparative Example 6 and Example 3 is that in Comparative Example 6, N-hydroxysuccinimide is replaced by N, N'-methylenebisacrylamide, the DPPH removal rate in Comparative Example 6 is 82.3%, the Escherichia coli sterilization rate is 85.1%, and the formaldehyde removal rate is 88.4%. Compared with Example 3, Comparative Example 6 has reduced antioxidant performance, antibacterial performance and formaldehyde removal ability; this is because N-hydroxysuccinimide is replaced by N, N'-methylenebisacrylamide, N, N'-methylenebisacrylamide is not easy to react with the amino group of the grafted tripeptide, the cross-linking of the antioxidant microcapsules and the grafted chitosan is reduced, and the stability of the fruity wood flavor for electronic cigarettes is reduced. Therefore, the antioxidant performance, antibacterial performance and formaldehyde removal ability of the fruity wood flavor for electronic cigarettes are all reduced.

[0119] This specific embodiment is merely an explanation of the present application and does not limit the present application. Based on the above description, relevant personnel can make various changes and modifications without departing from the technical scope of the present application. The technical scope of the present application is not limited to the contents of the specification and must be determined according to the scope of the claims.

Claims

1. A fruity wood flavor for electronic cigarettes, characterized by: The composition includes the following parts by weight: 10-15 servings of antioxidant microcapsules 15-25 parts grafted chitosan 3-5 parts surfactant 10-20 parts of cedar flavor essence; The antioxidant microcapsules include sodium alginate, a grafted tripeptide and a cross-linking agent; The grafted tripeptide includes methyl methacrylate functionalized dextran and His-Lys-Cys tripeptide (histidine-lysine-cysteine ​​tripeptide); The mass ratio of the sodium alginate, the grafted tripeptide and the cross-linking agent is 1: (0.5-0.8): 0.05; The cross-linking agent is tannic acid; The antioxidant microcapsules are prepared by the following steps: dissolving dextran, sodium hydroxide, and glycidyl methacrylate in anhydrous ethanol to obtain a reaction solution, neutralizing excess sodium hydroxide with hydrochloric acid after the reaction, dialyzing and freeze-drying the resulting solution to obtain methyl methacrylate-functionalized dextran; Dissolving His-Lys-Cys tripeptide, methyl methacrylate functionalized dextran and sodium hydroxide in phosphate buffer to obtain a mixed solution, vortexing the mixed solution, neutralizing excess sodium hydroxide with hydrochloric acid, desalting and purifying, and then freeze-drying to obtain a grafted tripeptide; The grafted tripeptide is dissolved in phosphate buffer to obtain a grafted tripeptide solution, sodium alginate and tannic acid are dissolved in deionized water to obtain a sodium alginate solution, the sodium alginate solution, Tween-80 and calcium chloride are added to the grafted tripeptide solution under stirring conditions to react, and the resulting solution is centrifuged and washed to obtain antioxidant microcapsules; The grafted chitosan comprises chitosan, chlorogenic acid amide and a coupling agent; The mass ratio of chitosan, chlorogenic acid amide and coupling agent is 1: (0.05-0.15): 0.05; The coupling agent is N-hydroxysuccinimide.

2. A process for preparing the fruity wood flavor for electronic cigarettes according to claim 1, characterized in that: The fruity wood flavor essence for electronic cigarettes is prepared by the following steps: dispersing cedar flavor essence and surfactant in deionized water to obtain emulsified flavor essence; dispersing antioxidant microcapsules and Tween-80 into emulsified flavor to obtain a dispersion; The grafted chitosan is added to the dispersion under stirring conditions, the pH is adjusted and then centrifuged to obtain a product, and the product is washed and dried to obtain the fruit wood flavor essence for electronic cigarettes.