CN112316862A - Preparation method of stevia rebaudiana enzyme microcapsule and application of stevia rebaudiana enzyme microcapsule in cigarettes - Google Patents
Preparation method of stevia rebaudiana enzyme microcapsule and application of stevia rebaudiana enzyme microcapsule in cigarettes Download PDFInfo
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- CN112316862A CN112316862A CN202011336582.2A CN202011336582A CN112316862A CN 112316862 A CN112316862 A CN 112316862A CN 202011336582 A CN202011336582 A CN 202011336582A CN 112316862 A CN112316862 A CN 112316862A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/302—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/043—Drying and spraying
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Abstract
The invention relates to a preparation method of stevia rebaudiana ferment microcapsules and application of the stevia rebaudiana ferment microcapsules in cigarettes. According to the invention, lactobacillus plantarum and bacillus subtilis are utilized for fermentation, so that the aftertaste of the spice can be improved, and the operation is simple; the extract is embedded by utilizing a microcapsule technology, so that the biological activity of the extract is maintained to the maximum extent, and the content of glucoside active ingredients of the extract is obviously improved; meanwhile, the loss of the aroma substances can be avoided, and the quality stability of the product is improved. After the microcapsule is applied to cigarettes, the release amount of harmful substances tar and CO in cigarette smoke can be reduced.
Description
Technical Field
The invention belongs to the technical field of tobacco flavors, and particularly relates to a stevia rebaudiana enzyme microcapsule extract. Meanwhile, the invention also relates to a preparation method of the tobacco flavor and application of the tobacco flavor in cigarettes.
Background
Stevia rebaudiana contains abundant glycosides, organic acids, amino acids, proteins, etc., and is named for its high sweetness and low calorie. The natural active substances contained in the stevia rebaudiana have important functions in the aspects of reducing blood sugar, reducing blood pressure, improving immunity, resisting oxidation, inhibiting bacteria and the like. At present, the application of stevia rebaudiana is mainly focused on related research of stevioside extraction. In the technical field of tobacco production, CN103783650A discloses an application of stevia rebaudiana in preparing reconstituted tobacco, which performs alcohol extraction treatment on stevia rebaudiana to obtain stevia rebaudiana extract and/or fiber for preparing reconstituted tobacco. However, the ethanol extraction of stevia rebaudiana can cause the loss of a part of effective components, and some pigments and other macromolecules in the extracting solution can be remained, thereby influencing the smoking taste of cigarettes. According to the invention, the stevia rebaudiana is compounded with various raw materials, so that the effects of the purslane, the dried loquat, the frankincense and the red raspberry are integrated, and the green grass smell of the stevia rebaudiana is improved. Meanwhile, the stevia rebaudiana compound is fermented and embedded in microcapsules for the first time, so that the glucoside active ingredients are retained to the maximum extent. The prepared microcapsule product is applied to cigarettes, so that the fragrance of the cigarettes can be increased on the basis of increasing the sweet feeling, and the harm of cigarette smoke can be reduced.
Disclosure of Invention
At present, the application of stevia rebaudiana in tobacco is mostly to extract stevioside, and the application of stevia rebaudiana in cigarettes is limited due to the fact that pigments are dissolved out in the stevia rebaudiana extracting process, and the woody gas is heavy. Meanwhile, the biological activity of the product is kept to the maximum extent by combining a microcapsule technology, and the convenience of storage and transportation of the product is improved. The application of the stevia rebaudiana bertoni extract in cigarettes obviously enhances the sweet and moist feeling of cigarette smoking, reduces the burning sensation and the pungent sensation of oral cavities and throats in the smoking process, simultaneously reduces the smoke hazard of the cigarettes, and is favorable for the comprehensive development and utilization of stevia rebaudiana bertoni.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the invention provides a preparation method of stevia rebaudiana ferment microcapsules, which comprises the following steps:
(1) pulverizing sweet stevia, adding distilled water and enzymolysis solution, soaking and hydrolyzing at 20-60 deg.C for 4-8 hr, inactivating enzyme, and filtering to obtain solution A;
(2) pulping the compound, and mixing to obtain a feed liquid B;
(3) mixing the feed liquid A and the feed liquid B, inoculating microorganisms, and fermenting at 30 deg.C for 7-14d to obtain fermentation liquid;
(4) filtering the fermentation liquor, adding petroleum ether into the filtrate, heating and refluxing at 30-60 deg.C, and concentrating to obtain concentrate;
(5) dissolving the concentrate with ethanol, refrigerating, centrifuging, removing insoluble substances and precipitate, and concentrating to obtain fermentation broth extract;
(6) freeze-drying the fermentation liquor extract until the water content is 3% -6%, and crushing to obtain fermentation product powder;
(7) dissolving the wall material in hot water at 80-100 ℃, adding the fermented product powder, adding 2% of emulsifier, stirring at high speed to form emulsified dispersion, and drying and curing by a spray dryer to obtain a microcapsule product;
wherein the compound in the step (2) is selected from one or more of purslane, dried loquat, frankincense and red raspberry.
Further, the enzymolysis liquid in the step (1) is selected from one or more of cellulase, laccase, pectinase and papain.
Further, the microorganism used in the step (3) is selected from one or more of lactobacillus plantarum, bacillus pumilus and bacillus subtilis.
Further, the centrifugation purification in the step (5) is centrifugation at <5000r/min for 15 min.
Further, in the step (6), the extract of the fermentation liquor is crushed to below 200 meshes.
Further, the wall material used in the step (7) is selected from one or more of beta-cyclodextrin, gum arabic, maltodextrin or gelatin.
Further, the wall material used in the step (7) is beta-cyclodextrin and gum arabic.
Furthermore, the concentration of the wall material is 0.1 g/mL-1 g/mL, and the weight ratio of the fermentation product powder to the wall material is 1: 6-1: 10.
The invention also provides an application method of the stevia rebaudiana ferment microcapsule obtained by the preparation method in cigarettes, which comprises the following steps: adding stevia rebaudiana ferment microcapsule into cigarette feed liquid, tobacco shred, cigarette paper or filter tip.
Further, the addition amount of the stevia rebaudiana enzyme microcapsule spice is 0.05-0.5% of the total weight of the tobacco shreds or the cigarette paper.
The application effects of the stevia rebaudiana ferment microcapsule product in cigarettes provided by the invention comprise: after the stevia rebaudiana ferment microcapsule is applied to cigarettes, the release amount of harmful substances, namely tar and CO in cigarette smoke can be reduced.
Compared with the existing research, the invention has the following advantages:
1. the invention provides the raw material compounding of the stevia rebaudiana enzyme, integrates the effects of purslane, dried loquat, frankincense and red raspberry, and improves the green grass smell of stevia rebaudiana;
2. firstly, stevia rebaudiana is used as a main raw material to carry out enzymolysis and fermentation, so that macromolecular substances are decomposed, and meanwhile, polysaccharide and other macromolecular substances which influence the smoking taste of the cigarettes are effectively removed by combining multi-stage purification, so that the stevia rebaudiana extract and the smoking taste of the cigarettes are coordinated;
3. microencapsulating the extract to maintain its biological activity to the maximum extent. After embedding, the content of glucoside active ingredients of the extract is obviously improved;
4. after the stevia rebaudiana enzyme microcapsule provided by the invention is applied to cigarettes, the release amount of harmful substances, namely tar and CO in cigarette smoke can be reduced.
The method has mild reaction conditions, simple equipment requirements and lower cost, is convenient for realizing large-scale industrial production, and the spice obtained by refluxing and alcohol precipitation has pure fragrance and pure product, and has stronger practicability and good development and application prospects. Meanwhile, the sweet feeling of cigarette smoking is obviously enhanced by combining the application in the cigarette, the burning sensation and the pungent sensation of the oral cavity and the throat in the smoking process are reduced, and the comprehensive development and utilization of the stevia rebaudiana are facilitated.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to specific examples.
Comparative example 1
(1) Pulverizing sweet stevia, adding distilled water and enzymolysis solution (pectase: laccase: cellulase 1:1:1), warm soaking at 45 deg.C for hydrolysis for 6 hr, and filtering to obtain solution A;
(2) uniformly mixing and pulping purslane, dried loquat, red raspberry and frankincense to obtain feed liquid B;
(3) mixing the feed liquid A and the feed liquid B, respectively activating lactobacillus plantarum and bacillus subtilis, inoculating into the mixed feed liquid, and fermenting at 30 ℃ for 7d to obtain fermentation liquid;
(4) filtering the fermentation liquor, taking the filtrate, adding petroleum ether, heating at 60 ℃, refluxing for extraction for 4h, and concentrating to obtain a concentrate;
(5) dissolving the concentrate with ethanol, refrigerating at 4 deg.C for 6 hr, centrifuging at 5000r/min for 10min, removing insoluble substances and precipitate, and concentrating to obtain fermentation broth extract.
Example 1
Preparation of microencapsulated stevia enzyme:
(1) freeze-drying the fermentation broth extract obtained in the comparative example 1 until the water content is 5%, crushing, and sieving with a 200-mesh sieve to obtain fermentation broth powder;
(2) dissolving beta-cyclodextrin and Arabic gum (weight ratio of beta-cyclodextrin to Arabic gum is 1:1.5) in hot water at 80 ℃, adding the crushed extract, wherein the wall material concentration is 0.5g/mL, and the core material: the wall material is 1:8, 2% of emulsifier is added, the mixture is stirred at high speed to form emulsified dispersion liquid, and the microcapsule product is obtained by drying and solidifying through a spray dryer.
Comparative example 2
(1) Pulverizing sweet stevia, adding distilled water and enzymatic hydrolysate (pectase: cellulase: 2:1), soaking and hydrolyzing at 45 deg.C for 6 hr, and filtering to obtain solution A;
(2) uniformly mixing and pulping purslane, dried loquat and frankincense to obtain feed liquid B;
(3) mixing the feed liquid A and the feed liquid B, respectively activating bacillus pumilus and bacillus subtilis, inoculating the mixture into the feed liquid, and fermenting at 30 ℃ for 7 days to obtain fermentation liquid;
(4) filtering the fermentation liquor, taking the filtrate, adding petroleum ether, heating at 60 ℃, refluxing for extraction for 4h, and concentrating to obtain a concentrate;
(5) dissolving the concentrate with ethanol, refrigerating at 4 deg.C for 7 hr, centrifuging at 5000r/min for 10min, removing insoluble substances and precipitate, and concentrating to obtain fermentation broth extract.
Comparative example 3
Comparative example 1 was repeated with the following differences: mixing the feed liquid A and the feed liquid B, then not carrying out inoculation fermentation, directly filtering, taking filtrate, adding petroleum ether, heating at 60 ℃, and carrying out reflux extraction for 4 hours. Concentrating, dissolving in ethanol, refrigerating at 4 deg.C for 12 hr, centrifuging at 5000r/min for 10min, removing insoluble substances and precipitate, and concentrating to obtain fermentation broth extract.
Comparative example 4
(1) Freeze-drying the fermentation broth extract obtained in comparative example 3 until the water content is 3%, crushing, and sieving with a 200-mesh sieve;
(2) dissolving beta-cyclodextrin and Arabic gum (weight ratio of beta-cyclodextrin to Arabic gum is 1:1.5) in hot water at 80 ℃, adding the crushed extract, wherein the wall material concentration is 0.6g/mL, and the core material: the wall material is 1:10, 1% of emulsifier is added, the mixture is stirred at high speed to form emulsified dispersion liquid, and the microcapsule product is obtained by drying and solidifying through a spray dryer.
Example 2
The preparation method is the same as that of example 1, except that the enzymolysis solution used is pectinase: papain 1:1.
Example 3
The preparation method is the same as that of example 1, except that the enzymolysis solution used is laccase: cellulase 2: 1.
Example 4
The preparation method was the same as in example 1 except that the microorganism used was Bacillus pumilus and Bacillus subtilis.
Example 5
The preparation method was the same as example 1 except that the microorganism used was Bacillus pumilus and Lactobacillus plantarum.
Example 6
The preparation method is the same as example 1, except that the wall materials used are maltodextrin and gelatin (2: 1).
Example 7
The preparation method is the same as example 1, except that the wall materials used are gum arabic and maltodextrin (1: 1).
Example 8
Analyzing the content of the glucoside substances: the fragrances obtained in examples 1 to 7 and comparative examples 1 to 4 were each tested for their glycoside content, and the results of the analysis are shown in Table 1.
TABLE 1 analysis of glycoside content results
Comparing comparative example 1, comparative example 3, comparative example 4 and example 1, it can be seen that the content of stevioside and rebaudioside a is increased after the compounded raw materials are fermented; compared with the products in comparative example 1, comparative example 2 and example 1, the content of the glycoside substances in the stevia rebaudiana composite extract is obviously improved after the stevia rebaudiana composite extract is embedded by the microcapsule.
Sensory evaluation: the flavors obtained in examples 1 to 7 and comparative examples 1 to 4 were subjected to cigarette sampling, and a control group was set to add an equal amount of distilled water. The smoking panel composed of smoking experts performs smoking evaluation, and the main evaluation indexes are coordination, aroma quality, irritation, aftertaste and the like. The fragrance quality is purer, fresh and attractive, and the impurity smell is less, wherein the higher the harmony and the fragrance quality score is, the better the harmony of the fragrance and the smoke is; the higher the irritation score is, the lower the smoke irritation is, the soft taste is obtained, the low score is, the choking of smoke nose is represented, and the irritation to throat is large; higher aftertaste scores represent longer persistence in the mouth and increased aftertaste. The sensory evaluation results of the cigarettes produced by sampling are shown in Table 2.
TABLE 2 average score of sensory evaluation results
Compared with the product and the blank sample, the spice prepared by the preparation method of the stevia rebaudiana essence disclosed by the invention can enter the oral cavity along with the smoke in the smoking process after being added into the cigarette tobacco shreds, so that the effect of the spice is fully exerted, the harmony and the fragrance quality of the cigarette can be properly increased, and the irritation is reduced; especially, after the compounded raw materials are fermented, the fragrance quality of the spice can be obviously improved; moreover, the product is added into the cigarette after microencapsulation, and compared with the flavor obtained by simple compound fermentation, the flavor has higher quality, lower irritation and better harmony and aftertaste when being added into the cigarette.
Example 9
Analysis of mainstream smoke: the mainstream smoke of the cigarette samples of the control group, examples 1 to 7 and comparative examples 1 to 4 was measured, and the results are shown in Table 3.
TABLE 3 analysis of mainstream Smoke
According to the analysis result of the mainstream smoke, the content of tar and CO in the smoke is reduced compared with that of a blank control group in the cigarette added with the stevia rebaudiana extract. Meanwhile, after the extract is microencapsulated, the effect of reducing the content of tar and CO in the cigarettes is more remarkable.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of stevia rebaudiana ferment microcapsules is characterized by comprising the following steps: the method comprises the following steps:
(1) pulverizing sweet stevia, adding distilled water and enzymolysis solution, soaking and hydrolyzing at 20-60 deg.C for 4-8 hr, inactivating enzyme, and filtering to obtain solution A;
(2) pulping the compound, and mixing to obtain a feed liquid B;
(3) mixing the feed liquid A and the feed liquid B, inoculating microorganisms, and fermenting at 30 deg.C for 7-14d to obtain fermentation liquid;
(4) filtering the fermentation liquor, adding petroleum ether into the filtrate, heating and refluxing at 30-60 deg.C, and concentrating to obtain concentrate;
(5) dissolving the concentrate with ethanol, refrigerating, centrifuging, removing insoluble substances and precipitate, and concentrating to obtain fermentation broth extract;
(6) freeze-drying the fermentation liquor extract until the water content is 3-6%, and crushing to obtain fermentation product powder;
(7) dissolving the wall material in hot water at 80-100 ℃, adding the fermented product powder, adding 2% of emulsifier, stirring at high speed to form emulsified dispersion, and drying and curing by a spray dryer to obtain a microcapsule product;
wherein the compound in the step (2) is selected from one or more of purslane, dried loquat, frankincense and red raspberry.
2. The method of claim 1, wherein: the enzymolysis liquid in the step (1) is selected from one or more of cellulase, laccase, pectinase and papain.
3. The method of claim 1, wherein: the microorganism used in the step (3) is one or more selected from lactobacillus plantarum, bacillus pumilus and bacillus subtilis.
4. The method of claim 1, wherein: the centrifugal purification in the step (5) is centrifugation for 15min at <5000 r/min.
5. The method of claim 1, wherein: in the step (6), the extract of the fermentation liquor is crushed to be below 200 meshes.
6. The method of claim 1, wherein: the wall material used in the step (7) is selected from one or more of beta-cyclodextrin, Arabic gum, maltodextrin or gelatin.
7. The method according to claim 1, characterized in that: the wall materials used in the step (7) are beta-cyclodextrin and Arabic gum.
8. The method of claim 1, wherein: the concentration of the wall material is 0.1 g/mL-1 g/mL, and the weight ratio of the fermentation product powder to the wall material is 1: 6-1: 10.
9. The application of the stevia rebaudiana ferment microcapsule obtained by the preparation method of any one of claims 1 to 8 in cigarettes is characterized in that the application method comprises the following steps: adding stevia rebaudiana ferment microcapsule into cigarette feed liquid, tobacco shred, cigarette paper or filter tip.
10. The method of application according to claim 9, characterized in that: the addition amount of the stevia rebaudiana enzyme microcapsule spice is 0.05-0.5% of the total weight of the tobacco shreds or the cigarette paper.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102217795A (en) * | 2010-04-19 | 2011-10-19 | 红塔烟草(集团)有限责任公司 | Preparation of microcapsule humectant and application thereof to cigarette |
| CN105661626A (en) * | 2016-03-25 | 2016-06-15 | 河南中烟工业有限责任公司 | Composite biological agent microcapsule capable of improving sensory quality of tobacco |
| CN109173948A (en) * | 2018-09-27 | 2019-01-11 | 上海烟草集团有限责任公司 | A kind of slow-release microcapsule material and its preparation method and application discharging fragrance |
| CN109999736A (en) * | 2019-04-24 | 2019-07-12 | 东莞市枭森环保科技有限公司 | A kind of microcapsules and preparation method thereof containing plant characteristics fragrance |
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- 2020-11-25 CN CN202011336582.2A patent/CN112316862B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102217795A (en) * | 2010-04-19 | 2011-10-19 | 红塔烟草(集团)有限责任公司 | Preparation of microcapsule humectant and application thereof to cigarette |
| CN105661626A (en) * | 2016-03-25 | 2016-06-15 | 河南中烟工业有限责任公司 | Composite biological agent microcapsule capable of improving sensory quality of tobacco |
| CN109173948A (en) * | 2018-09-27 | 2019-01-11 | 上海烟草集团有限责任公司 | A kind of slow-release microcapsule material and its preparation method and application discharging fragrance |
| CN109999736A (en) * | 2019-04-24 | 2019-07-12 | 东莞市枭森环保科技有限公司 | A kind of microcapsules and preparation method thereof containing plant characteristics fragrance |
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