CN117158630A

CN117158630A - Preparation method of characteristic-flavor electronic cigarette liquid microcapsule

Info

Publication number: CN117158630A
Application number: CN202311170216.8A
Authority: CN
Inventors: 祖萌萌; 许红涛; 李华雨; 王艳青; 李晓瑜; 王茹楠; 常岭; 薛建中
Original assignee: Henan Cigarette Industrial Tobacco Slice Co ltd
Current assignee: Henan Cigarette Industrial Tobacco Slice Co ltd
Priority date: 2023-09-12
Filing date: 2023-09-12
Publication date: 2023-12-05

Abstract

The application discloses a preparation method of a characteristic-flavor electronic cigarette liquid microcapsule, which comprises the steps of carrying out enzymolysis on proteins in tobacco leaves to amino acid, hydrolyzing starch to glucose, maltose and the like, extracting and concentrating, adding reducing sugar and amino acid into tobacco leaf extract and waxberry extract to carry out Maillard reaction, and preparing Maillard reactants into microcapsule emulsion.

Description

Preparation method of characteristic-flavor electronic cigarette liquid microcapsule

Technical Field

The application belongs to the technical field of electronic cigarette production, and particularly relates to a preparation method of a characteristic-flavor electronic cigarette liquid microcapsule.

Background

The electronic cigarette generates the smokeable aerosol by heating the tobacco liquid under the control of the electronics, has the advantages of no combustion, no harm of second-hand smoke and the like, and has wide market prospect. Electronic cigarettes have various tastes, and smoke liquid is generally transparent or semitransparent, so that the electronic cigarettes are rich in color and meet the requirements of different consumers. With further standardization of the tobacco industry, the admission of non-tobacco style electronic cigarettes is tightened, and the commercial electronic cigarettes inevitably return to the tobacco taste style.

At present, tobacco source substances added in the electronic tobacco juice are mainly tobacco essential oil and tobacco bud oil, and the oil can keep the physical properties of the tobacco juice while giving the tobacco style, but also cause the phenomenon of poor smoking taste, mainly because the essential oil and the bud oil are mainly volatile tobacco head fragrance substances and can not express the complete fragrance style of tobacco.

The tobacco extract is used as another tobacco reprocessing product, water or ethanol is generally adopted as a solvent, wherein the extraction rate is generally more than 90% after the water extraction is carried out alone, and the obtained extract can have more comprehensive tobacco style characteristics. However, the application of the extract in the electronic cigarette liquid is limited, on one hand, because macromolecular substances such as sugar, protein and starch in the extract are easy to precipitate, the appearance of the cigarette liquid is poor, and on the other hand, the burnt smell generated by the substances reacts in the heating process of the electronic cigarette, so that the smoking sensory quality is poor, the atomization capability and the atomization effect of the electronic cigarette are also influenced, and further application of the tobacco extract is limited.

The tobacco extract has wide sources of raw materials, mainly comprises fragments, tobacco powder and tobacco leaves, wherein the tobacco leaves are mainly caused by low grade of the tobacco leaves or unsuitable tobacco processing due to unbalance of chemical components of the tobacco leaves, and generally have negative influences such as combustibility, miscellaneous gases, irritation and the like. Thus, the rational use of tobacco leaves is currently still an important direction of research in the tobacco industry.

The red-brown paste is obtained by drying, fermenting, crushing, extracting with water or extracting with alcohol, has typical strong sweet fruit fragrance, and is an important additive for cigarettes. Volatile components of the waxberry extract can endow the product with unique waxberry alcoholization characteristics in the electronic cigarette, and enrich the tobacco fragrance; however, the main components in the waxberry extract, such as a large amount of sugar substances and amino acids, do not have the application effects of the traditional cigarettes, such as fragrance enrichment, irritation relief, alcohol and smoke reduction and the like. The Maillard reaction product contains a large amount of aroma components which are coordinated with tobacco, has the advantages of strong natural feel, full aroma and the like, and has good application effect in improving the quality of tobacco products, so that the Maillard reaction becomes an important way for preparing tobacco flavor. The microcapsule technology is to embed small droplets, solid particles, etc. in a microcapsule wall material to become flowable particles. The microencapsulation can prevent volatilization loss of the core material in the storage process and ensure uniform release of the core material.

There are some related patents related to microcapsule technology for preparing electronic cigarette liquid. As patent CN201410402403.9 discloses an electronic cigarette with microcapsule slow release device and microcapsule, through microcapsule of tobacco juice, environmental contact is isolated, components of tobacco juice are not polluted, and different tastes can be felt. Patent CN202111036865.X discloses a microcapsule for electronic cigarette liquid, wherein the wall material is beta-cyclodextrin or hydroxypropyl-beta-cyclodextrin, and the core material is tobacco essential oil. Patent CN201810929445.6 provides an electronic cigarette liquid, which uses cyclodextrin as a capsule wall, uses essence and nicotine as core materials, and prepares the essence and the nicotine into microcapsule type electronic cigarette liquid. However, no report on the application of the Maillard reactants of tobacco leaves and waxberries to electronic cigarettes after microencapsulation is known at present. Based on this, the present application has been developed.

Disclosure of Invention

The application aims to overcome the defects of the prior art and provide a preparation method of characteristic-flavor electronic cigarette liquid microcapsules, which utilizes a large amount of protein and carbohydrate contained in tobacco leaves and waxberry extract to further prepare tobacco fragrances with rich fragrance and higher fragrance quality through Maillard reaction and prepares the electronic cigarette liquid microcapsules by embedding the tobacco fragrances through a microcapsule technology, so that the tobacco waste is reduced, and meanwhile, the prepared electronic cigarette liquid microcapsules not only have strong tobacco fragrance and characteristic fragrance of waxberries, but also increase characteristic fragrance of Maillard reaction products, and have long shelf life, good stability and uniform and stable smoke release during suction.

In order to achieve the above purpose, the application adopts the following technical scheme:

the preparation method of the characteristic-flavor electronic cigarette liquid microcapsule specifically comprises the following steps:

1) Adding pectase, protease and amylase into tobacco leaves for enzymolysis, extracting the tobacco leaves after enzymolysis with water, centrifuging the extracting solution, separating the extracting solution by a membrane, and concentrating the extracting solution into tobacco extract under negative pressure;

2) Uniformly mixing tobacco extract, waxberry extract, reducing sugar, amino acid and solvent, regulating the pH value of a reaction system to 7-10, supplementing water until the water content in the system is 12% -15%, uniformly stirring, controlling the temperature of the system to 90-150 ℃ for reaction for 1-3h, cooling, centrifuging and removing impurities to obtain a Maillard reactant;

3) Dissolving microcapsule coating raw materials with water, slowly adding Maillard reactants, dispersing the mixture at high speed to obtain emulsion microcapsule, spray drying to obtain electronic cigarette liquid microcapsule, or preparing microcapsule by conventional method. The obtained electronic cigarette has rich tobacco fragrance and characteristic fragrance of waxberry, and has long shelf life, good stability, and uniform and stable fragrance release during suction.

Specifically, in the step 1), the addition amount of pectase, protease and amylase is 0.1-0.8% of the tobacco leaf mass.

Further, in the step 1), the enzymolysis temperature may be 40-50 ℃ and the enzymolysis time may be 5-12 hours.

Further, in the step 1), water which is 5-10 times of the tobacco leaf quality can be added into the tobacco leaf subjected to enzymolysis for extraction, the extraction temperature is 50-75 ℃, and the extraction time is 1-2.5 hours. During membrane separation, a silicon carbide tubular membrane with the aperture of 0.05-2.0 mu m can be selected, and substances with the molecular weight of 20 ten thousand-100 ten thousand, and suspended impurities such as microfibers, particles and the like are mainly retained.

Specifically, in the step 2), the reducing sugar may be one or a mixture of more than two of xylose, arabinose, glucose, fructose, mannose, galactose and the like; the amino acid can be one or more of proline, leucine, tryptophan, threonine, serine, phenylalanine and the like.

Further, in step 2), the solvent may be one or a mixture of two or more of propylene glycol, glycerin, ethylene glycol, and the like.

Specifically, in the step 2), 20 parts of tobacco extract, 20-30 parts of waxberry extract, 10-15 parts of reducing sugar, 0.6-2.0 parts of amino acid and 17-20 parts of solvent can be uniformly mixed according to parts by weight.

Further, in the step 2), when the pH value of the reaction system is adjusted, the acidic compound may be one or more of edible hydrochloric acid, acetic acid, citric acid, etc., and the alkaline compound may be one or more of ammonia water, na0H, KOH, etc.

Further, in step 3), the microcapsule coating raw material may include one or a mixture of two or more of polyvinyl alcohol, cyclodextrin, guar gum, cellulose derivative, and the like. After the microcapsule coating raw material is dissolved by water, a microcapsule coating raw material solution with the mass concentration of 2-8% is obtained, and the mass ratio of the microcapsule coating raw material solution to the Maillard reactant is 1: 5-10.

Compared with the prior art, the preparation method has the following beneficial effects:

the electronic cigarette liquid microcapsule prepared by the method has the characteristics of rich tobacco fragrance and waxberry fragrance, increases the characteristic fragrance of Maillard reaction products, and has long shelf life, good stability and uniform and stable smoke release during suction. In addition, the application has mild reaction conditions, relatively simple required equipment and easy industrialized production.

Detailed Description

The following describes the technical scheme of the present application in further detail with reference to examples, but the scope of the present application is not limited thereto.

In the examples below, the starting materials used are either commercially available products which are commercially available as such or are prepared by methods conventional in the art. For example, the pectase and amylase manufacturers are Shandong Hoverbut enzyme preparation limited, the pectase activity is 30000u/g, and the amylase activity is 50000 u/g; the protease manufacturer is the biological engineering Co., ltd of Nanning Pang Bo, and the protease activity is 200000 u/g.

In the examples, unless otherwise specified, the operations or processes involved are all within the skill of the art.

Example 1

1) Adding enzymolysis solution prepared from pectase, protease and amylase into tobacco leaf, performing enzymolysis reaction, and extracting the tobacco leaf after enzymolysis with water. Wherein the addition amounts of pectase, protease and amylase are respectively 0.2%, 0.2% and 0.5% of the tobacco leaf mass. The enzymolysis temperature is 40 ℃ and the enzymolysis time is 6 hours. Adding water with the mass of 5 times of that of the tobacco leaves into the tobacco leaves subjected to enzymolysis for extraction, wherein the extraction temperature is 50 ℃ and the extraction time is 1.5h;

2) Centrifuging the extractive solution, and separating with silicon carbide tubular membrane (JMtech-SICT-30-4-19-1016, model number of Zhejiang firm membrane technology Co., ltd.) with pore diameter of 1.0 μm;

3) Concentrating the extracting solution into tobacco extract under negative pressure, uniformly mixing the tobacco extract and the commercial ethanol-extracted waxberry extract (purchased from Zhengzhou Jieshi chemical industry Co., ltd.) with reducing sugar, amino acid and solvent, regulating the pH value of the reaction system to 7, supplementing water until the water content in the system is 12%, uniformly stirring, controlling the reaction temperature of the system to 100 ℃, controlling the reaction time to 1h, and centrifuging to remove impurities after cooling to obtain the Maillard reactant. Wherein the solvent is propylene glycol, and the reducing sugar is glucose and fructose with a mass ratio of 3:1. The amino acids are proline, leucine, threonine and phenylalanine in a mass ratio of 1:2:2:2. When the tobacco extract is 20 parts by mass, the waxberry extract is 20 parts by mass, the reducing sugar is 10 parts by mass, the amino acid is 0.6 part by mass, and the solvent is 18 parts by mass. The compound adopted for regulating the pH value of the reaction system is ammonia water;

4) Slowly adding polyvinyl alcohol into water, heating to 90 ℃ and stirring for dissolution (the concentration of the polyvinyl alcohol solution is about 5%), and slowly adding Maillard reactant (the mass ratio of the polyvinyl alcohol solution to the Maillard reactant is 1:10 And (3) performing high-speed dispersion on the mixture to obtain emulsion microcapsules, and performing spray drying to obtain the required electronic cigarette liquid microcapsules.

The control sample is tobacco juice, and the specific preparation process is as follows: the first two steps are the same as in example 1, then the extracting solution is concentrated into tobacco extract under negative pressure, and the tobacco extract, the waxberry extract extracted by commercial ethanol and the propylene glycol are uniformly mixed according to the mass parts of 20:20:18, so that the control tobacco liquid is obtained.

And weighing the electronic cigarette liquid microcapsule, observing the change of the quality of the electronic cigarette liquid microcapsule along with the standing time, and researching the slow release performance of the tobacco microcapsule.

TABLE 1 quality variation of Smoke microcapsules with time of placement

Note that: the control sample was left for 205 days with an equivalent amount of smoke liquid (0.6400 g) to evaporate completely.

As can be seen from table 1 above: the tobacco juice microcapsule of the embodiment 1 of the application has the retention rate of 91.53% after being placed for 240 days, and the equivalent tobacco juice of the control sample is completely volatilized after being placed for 205 days, so that the tobacco juice microcapsule has better stability and longer preservation time than the independent tobacco juice.

Please the expert to evaluate the suction, the sensory quality evaluation sets the items and scores as follows: the amount of smoke was 10 minutes, the aroma was 30 minutes, the harmony was 10 minutes, the irritation was 10 minutes, the miscellaneous gas was 20 minutes, the aftertaste was 20 minutes, the total score was 100 minutes, and the absorption results are shown in Table 2.

Table 2 sensory quality evaluation

As can be seen from table 2 above: the samples of the application in example 1 have higher sensory quality scores than the control samples, such as aroma and coordination, and the total score is 5.5 minutes higher than the control samples. Meanwhile, the sample of the embodiment 1 releases more evenly and stably smoke, and has strong typical tobacco fragrance and waxberry characteristic fragrance style.

Example 2

1) Adding enzymolysis solution prepared from pectase, protease and amylase into tobacco leaf, performing enzymolysis reaction, extracting the tobacco leaf after enzymolysis with water, and concentrating under negative pressure to obtain tobacco extract. Wherein the addition amounts of pectase, protease and amylase are respectively 0.1%, 0.3% and 0.5% of the tobacco leaf mass. The enzymolysis temperature is 45 ℃ and the enzymolysis time is 5 hours. Adding water with the mass of 6 times of that of the tobacco leaves into the tobacco leaves subjected to enzymolysis for extraction, wherein the extraction temperature is 60 ℃ and the extraction time is 2.0h;

2) Centrifuging the extract and separating the extract by using a silicon carbide tubular membrane with a pore diameter of 0.5 μm;

3) Concentrating the extracting solution into tobacco extract under negative pressure, uniformly mixing the tobacco extract and the waxberry extract extracted by ethanol sold in the market with reducing sugar, amino acid and solvent, regulating the pH value of a reaction system to 8, supplementing water until the water content in the system is 12%, uniformly stirring, controlling the reaction temperature of the system to 95 ℃, controlling the reaction time to 2 hours, and centrifuging to remove impurities after cooling to obtain the Maillard reactant. Wherein the solvent is propylene glycol or glycerol. The reducing sugar is arabinose and glucose with the mass of 1:2. The amino acids are proline, threonine, serine and phenylalanine in a mass ratio of 2:1:1:2. When the tobacco extract is 20 parts by mass, the waxberry extract is 20 parts by mass, the reducing sugar is 15 parts by mass, the amino acid is 1.0 part by mass, and the solvent is 20 parts by mass. The compound adopted for regulating the pH value of the reaction system is Na0H;

4) Cyclodextrin is slowly added into water, heated to 60 ℃ and stirred for dissolution (the concentration of the cyclodextrin solution is about 2%), and then maillard reactant is slowly added (the mass ratio of the cyclodextrin solution to the maillard reactant is 1: 8) And (3) dispersing the mixture at a high speed to obtain emulsion microcapsules, and spray-drying to obtain the required electronic cigarette liquid microcapsules.

Example 3

1) Adding enzymolysis solution prepared from pectase, protease and amylase into tobacco leaf, performing enzymolysis reaction, extracting the tobacco leaf after enzymolysis with water, and concentrating under negative pressure to obtain tobacco extract. Wherein the addition amounts of pectase, protease and amylase are respectively 0.4%, 0.4% and 0.3% of the tobacco leaf mass. The enzymolysis temperature is 50 ℃ and the enzymolysis time is 8 hours. Adding water with the mass of 8 times of that of the tobacco leaves into the tobacco leaves subjected to enzymolysis for extraction, wherein the extraction temperature is 70 ℃ and the extraction time is 2.5h;

3) Concentrating the extracting solution into tobacco extract under negative pressure, uniformly mixing the tobacco extract and the waxberry extract extracted by ethanol sold in the market with reducing sugar, amino acid and solvent, regulating the pH value of a reaction system to be 10, supplementing water until the water content in the system is 12%, uniformly stirring, controlling the reaction temperature of the system to be 120 ℃, controlling the reaction time to be 3 hours, and centrifuging to remove impurities after cooling to obtain the Maillard reactant. Wherein the solvent is glycerol and the reducing sugar is glucose. The amino acids are a mixture of proline, leucine, tryptophan and serine in a mass ratio of 2:1:1:1. When the mass part of the tobacco extract is 20, the mass part of the waxberry extract is 25, the mass part of the reducing sugar is 10, the mass part of the amino acid is 2.0 and the mass part of the solvent is 18. The compound adopted for regulating the pH value of the reaction system is K0H;

4) Slowly adding polyvinyl alcohol into water, heating to 90 ℃ and stirring for dissolution (the concentration of the polyvinyl alcohol solution is about 4%), and slowly adding Maillard reactant (the mass ratio of the polyvinyl alcohol solution to the Maillard reactant is 1: 6) And (3) dispersing the mixture at a high speed to obtain emulsion microcapsules, and spray-drying to obtain the required electronic cigarette liquid microcapsules.

The smoke microcapsules of examples 2 and 3 were evaluated for sensory quality, and the evaluation results were comparable to those of example 1.

The foregoing is merely illustrative embodiments of the present application, and the present application is not limited thereto, and any changes or substitutions that may be easily contemplated by those skilled in the art within the scope of the present application should be included in the scope of the present application. Therefore, the protection scope of the present application should be subject to the protection scope of the claims.

Claims

1. The preparation method of the characteristic-flavor electronic cigarette liquid microcapsule is characterized by comprising the following steps of:

3) After the microcapsule coating raw materials are dissolved, maillard reactants are added for dispersion, emulsion microcapsules are obtained, and the emulsion microcapsules are spray-dried, so that the electronic cigarette liquid microcapsules are obtained, or the microcapsules are prepared according to the conventional method.

2. The method for preparing the characteristic-flavor electronic cigarette liquid microcapsule according to claim 1, wherein in the step 1), the addition amount of pectase, protease and amylase is 0.1-0.8% of the mass of tobacco leaves.

3. The method for preparing characteristic-flavor electronic cigarette liquid microcapsules according to claim 1, wherein in the step 1), the enzymolysis temperature is 40-50 ℃ and the enzymolysis time is 5-12h.

4. The method for preparing the characteristic-flavor electronic cigarette liquid microcapsule according to claim 1, wherein in the step 1), water which is 5-10 times of the mass of tobacco leaves is added into the tobacco leaves subjected to enzymolysis for extraction, the extraction temperature is 50-75 ℃, and the extraction time is 1-2.5 hours.

5. The method for preparing characteristic-flavor electronic cigarette liquid microcapsules according to claim 1, wherein in the step 2), the reducing sugar is one or a mixture of more than two of xylose, arabinose, glucose, fructose, mannose and galactose; the amino acid is one or more of proline, leucine, tryptophan, threonine, serine and phenylalanine.

6. The method for preparing characteristic-flavor electronic cigarette liquid microcapsules according to claim 1, wherein in the step 2), the solvent is one or a mixture of more than two of propylene glycol, glycerin and ethylene glycol.

7. The method for preparing characteristic-flavor electronic cigarette liquid microcapsules according to claim 1, wherein in the step 2), 20 parts of tobacco extract, 20-30 parts of waxberry extract, 10-15 parts of reducing sugar, 0.6-2.0 parts of amino acid and 17-20 parts of solvent are uniformly mixed in parts by weight.

8. The method for preparing characteristic-flavor electronic cigarette liquid microcapsules according to claim 1, wherein in the step 2), when the pH value of the reaction system is adjusted, the acidic compound is one or more of edible hydrochloric acid, acetic acid and citric acid, and the alkaline compound is one or more of ammonia water and Na0H, KOH.

9. The method for preparing characteristic-flavor electronic cigarette liquid microcapsules according to claim 1, wherein in the step 3), the microcapsule coating raw material comprises one or a mixture of more than two of polyvinyl alcohol, cyclodextrin, guar gum and cellulose derivatives.