CN109007955B - Tobacco stem extract, preparation method thereof and tobacco product - Google Patents
Tobacco stem extract, preparation method thereof and tobacco product Download PDFInfo
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- CN109007955B CN109007955B CN201810645182.6A CN201810645182A CN109007955B CN 109007955 B CN109007955 B CN 109007955B CN 201810645182 A CN201810645182 A CN 201810645182A CN 109007955 B CN109007955 B CN 109007955B
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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
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
Abstract
The invention provides a tobacco stem extract, a preparation method thereof and a tobacco product. The preparation method of the tobacco stem extract provided by the invention comprises the following steps: a) mixing and heating tobacco stems and water to obtain tobacco stem liquid; mixing and activating the complex enzyme and water to obtain an enzyme dispersion liquid; the complex enzyme comprises cellulase, pectinase, xylanase, protease, amylase and glucoamylase; b) mixing the tobacco stalk liquid and an enzyme dispersion liquid, and heating for reaction to obtain a reactant; c) carrying out alcohol extraction on the reactant to obtain an extracting solution; d) reacting the extracting solution with a compound additive to obtain a tobacco stem extract; the compound additive comprises cellulase, xylose, fructose and vitamin C. The preparation method provided by the invention can effectively remove negative taste substances in the tobacco stems, which influence the taste of smoking, can promote substance conversion, increase a large amount of fragrant substances with tobacco aroma, and greatly improve the smoking quality of tobacco products.
Description
Technical Field
The invention relates to the technical field of tobacco, in particular to a tobacco stem extract, a preparation method thereof and a tobacco product.
Background
Tobacco is an annual herbaceous plant in solanaceae, is one of economic crops with the widest global distribution and the largest planting area, and is mainly used for producing tobacco products such as cigarettes. Due to the extremely high economic value, the cigarette industry is driven to become the economic support industry of many countries. Besides tobacco raw materials, tobacco flavors and fragrances of various formulas are also indispensable components in the cigarette production process. However, these artificial essences easily generate offensive odor, lack natural feeling, and affect cigarette quality.
In order to solve the above problems, most of the tobacco products have been added to tobacco as a flavor or essential oil to simulate the feeling of aroma and flavor of cigarettes. For example, in the prior art, the tobacco stem extract is used as the tobacco absolute oil or the flavor, so that the tobacco waste such as the tobacco stems is recycled, and the defects of artificial flavor can be overcome.
At present, the prior art mainly comprises a steam distillation method and a solvent extraction method for preparing the tobacco stem extract. In the steam distillation method, as compared with tobacco stems and tobacco leaves in terms of composition, lignin, cellulose and other negative flavor absorbing substances which affect the taste of smoking are more, and aroma components are less, the steam distillation method is adopted to have poor extraction efficiency and extraction effect on the tobacco stems, so that the aroma components cannot be extracted well, and more impurities affect the smoking quality; meanwhile, the steam distillation method needs high heating temperature, so that heat-sensitive fragrant substances are lost along with steam evaporation, and further, less fragrant substances and less vivid fragrance are caused. Although the solvent extraction method has high yield, the extraction effect is poor, the extract contains a large amount of impurities such as resin, wax and the like, the aroma function of the extract is influenced, the smoking quality is further influenced, the extract needs to be further refined, the process is very complicated, the large-scale production is difficult to realize, and the method has the problem of recycling the organic solvent and has adverse effect on the environment.
Disclosure of Invention
In view of the above, the invention aims to provide a tobacco stem extract, a preparation method thereof and a tobacco product, the preparation method of the tobacco stem extract provided by the invention can effectively remove impurities in the tobacco stem which affect the taste of smoking, improve the purity of the extract, effectively increase the flavor substances with tobacco roasting flavor, and greatly improve the smoking quality; the preparation method is simple and easy to implement, does not need complex equipment or harsh conditions, and is favorable for realizing large-scale production.
The invention provides a preparation method of a tobacco stem extract, which comprises the following steps:
a) mixing and heating tobacco stems and water to obtain tobacco stem liquid;
mixing and activating the complex enzyme and water to obtain an enzyme dispersion liquid;
the complex enzyme comprises cellulase, pectinase, xylanase, protease, amylase and glucoamylase;
b) mixing the tobacco stalk liquid and an enzyme dispersion liquid, and heating for reaction to obtain a reactant;
c) carrying out alcohol extraction on the reactant to obtain an extracting solution;
d) reacting the extracting solution with a compound additive to obtain a tobacco stem extract;
the compound additive comprises cellulase, xylose, fructose and vitamin C.
Preferably, in the compound enzyme, the mass ratio of cellulase, pectinase, xylanase, protease, amylase and glucoamylase is (0.08-0.12): (0.18-0.22): (0.08-0.12): (0.20-0.24): (0.18-0.22): (0.08-0.12);
the mass ratio of the complex enzyme to the tobacco stems is (0.80-1.04) to 100.
Preferably, in the step b), the heating reaction is carried out at the temperature of 45-55 ℃ for 6-7 hours.
Preferably, in the compound additive, the mass ratio of the cellulase to the xylose to the fructose to the vitamin C is (0.18-0.22) to (0.28-0.32) to (0.04-0.06) to (0.18-0.22);
the mass ratio of the composite additive to the tobacco stems is (0.68-0.82) to 100.
Preferably, in the step d), the reaction temperature is 90-100 ℃ and the reaction time is 2.5-3.5 h.
Preferably, in the step a), when the tobacco stems and the water are mixed and heated, the mass ratio of the tobacco stems to the water is 100 to (650-900); the mixing and heating temperature is 45-55 ℃, and the time is 25-35 min;
when the complex enzyme and water are mixed and activated, the mass ratio of the complex enzyme to the water is (0.80-1.04) to (30-50); the temperature of mixing activation is 20-30 ℃, and the time is 15-25 min.
Preferably, the step c) comprises:
c1) mixing and heating the reactant and ethanol, and carrying out solid-liquid separation to obtain filtrate and filter residue;
c2) mixing the filtrate with propylene glycol, and concentrating to obtain extractive solution.
Preferably, the step c1) includes:
c1-1) mixing the reactant with ethanol, heating, and carrying out solid-liquid separation to obtain a first filtrate and filter residue;
c1-2) mixing and heating the filter residue and ethanol, and carrying out solid-liquid separation to obtain a second filtrate;
c1-3) combining the first filtrate with the second filtrate to obtain a filtrate.
The invention provides a tobacco stem extract prepared by the preparation method in the technical scheme.
The invention provides a tobacco product which comprises the tobacco stem extract in the technical scheme.
The invention provides a preparation method of a tobacco stem extract, which comprises the following steps: a) mixing and heating tobacco stems and water to obtain tobacco stem liquid; mixing and activating the complex enzyme and water to obtain an enzyme dispersion liquid; the complex enzyme comprises cellulase, pectinase, xylanase, protease, amylase and glucoamylase; b) mixing the tobacco stalk liquid and an enzyme dispersion liquid, and heating for reaction to obtain a reactant; c) carrying out alcohol extraction on the reactant to obtain an extracting solution; d) reacting the extracting solution with a compound additive to obtain a tobacco stem extract; the compound additive comprises cellulase, xylose, fructose and vitamin C. The preparation method provided by the invention can effectively remove negative taste substances in the tobacco stems, which influence the taste of smoking, can promote substance conversion, increase a large amount of fragrant substances with tobacco aroma, and greatly improve the smoking quality of tobacco products.
Detailed Description
The invention provides a preparation method of a tobacco stem extract, which comprises the following steps:
a) mixing and heating tobacco stems and water to obtain tobacco stem liquid;
mixing and activating the complex enzyme and water to obtain an enzyme dispersion liquid;
the complex enzyme comprises cellulase, pectinase, xylanase, protease, amylase and glucoamylase;
b) mixing the tobacco stalk liquid and an enzyme dispersion liquid, and heating for reaction to obtain a reactant;
c) carrying out alcohol extraction on the reactant to obtain an extracting solution;
d) reacting the extracting solution with a compound additive to obtain a tobacco stem extract;
the compound additive comprises cellulase, xylose, fructose and vitamin C.
The preparation method provided by the invention can effectively remove negative taste substances in the tobacco stems, which influence the taste of smoking, can promote substance conversion, increase a large amount of fragrant substances with tobacco aroma, and greatly improve the smoking quality of tobacco products.
According to the invention, tobacco stems and water are mixed and heated to obtain tobacco stem liquid.
In the invention, the tobacco stems are the waste tobacco stems. The tobacco stems are preferably tobacco stem powder, namely, waste tobacco stem shreds are crushed into powder. The crushing mode is not particularly limited, and the tobacco stems can be crushed, for example, the tobacco stems can be crushed by an agricultural straw crusher. In the present invention, it is preferable that the tobacco stalk powder is further sieved after the pulverization, and the tobacco stalk powder having a certain particle size is selected as a raw material. In the invention, the granularity of the tobacco stalk powder is preferably 40-60 meshes.
In the invention, the mass ratio of the tobacco stems to the water is preferably 100 to (650-900), and more preferably 100 to (700-800). The mixing and heating temperature is preferably 45-55 ℃; the mixing and heating time is preferably 25-35 min, and tobacco stem liquid is obtained after the mixing and heating treatment.
According to the invention, the complex enzyme is mixed with water for activation to obtain the enzyme dispersion.
In the invention, the complex enzyme comprises cellulase, pectinase, xylanase, protease, amylase and glucoamylase; the source of the complex enzyme component is not particularly limited, and the complex enzyme component is a general commercial product. In the compound enzyme, the mass ratio of cellulase, pectinase, xylanase, protease, amylase and glucoamylase is preferably (0.08-0.12) to (0.18-0.22) to (0.08-0.12) to (0.20-0.24) to (0.18-0.22) to (0.08-0.12). In the invention, the mass ratio of the complex enzyme to the tobacco stems is preferably (0.80-1.04) to 100. More preferably, the mass ratio of the cellulase to the tobacco stems is (0.08-0.12) to 100; the mass ratio of the pectinase to the tobacco stems is (0.18-0.22) to 100; the mass ratio of the xylanase to the tobacco stems is (0.08-0.12) to 100; the mass ratio of the protease to the tobacco stems is (0.20-0.24) to 100; the mass ratio of the amylase to the tobacco stems is (0.18-0.22) to 100; the mass ratio of the saccharifying enzyme to the tobacco stems is (0.08-0.12) to 100.
In the invention, when the compound enzyme is mixed with water, the mass ratio of the compound enzyme to the water is preferably (0.80-1.04): (30-50). In the invention, the mixing and activating temperature is preferably 20-30 ℃; the mixing and activating time is preferably 15-25 min; after the mixing activation, an enzyme dispersion was obtained.
The invention has no restriction on the order of obtaining the tobacco stalk liquid and the enzyme dispersion liquid.
According to the invention, after the tobacco stem liquid and the enzyme dispersion liquid are obtained, the tobacco stem liquid and the enzyme dispersion liquid are mixed and heated for reaction, and a reactant is obtained.
In the invention, the heating reaction temperature is preferably 45-55 ℃. The heating reaction time is preferably 6-7 h. The tobacco stalk liquid and the enzyme dispersion liquid carry out enzymatic reaction, so that the effects of wall breaking, quality improvement and impurity removal are achieved, the wall breaking, the impurity removal and the macromolecular substance conversion can be effectively and rapidly realized, and the purity of the extract is improved. In contrast, the traditional extraction methods such as solvent extraction and the like can generate a large amount of residues and generate negative effects such as rough smoke and the like, and the specific enzymatic reaction is carried out, so that the problems can be overcome, and the effects of removing impurities and improving fragrance can be achieved.
According to the invention, after the reactant is obtained, the reactant is subjected to alcohol extraction to obtain an extracting solution.
Preferably, the method specifically comprises the following steps:
c1) mixing and heating the reactant and ethanol, and carrying out solid-liquid separation to obtain filtrate and filter residue;
c2) mixing the filtrate with propylene glycol, and concentrating to obtain extractive solution.
In the step c1), the mass percentage concentration of the ethanol is preferably 92-98%. The mass ratio of the ethanol to the initial tobacco stems is preferably (400-450) to 100. The mixing and heating temperature is preferably 85-95 ℃; the mixing and heating time is preferably 0.8-1.2 h.
After the mixing and heating, solid-liquid separation is performed. The solid-liquid separation mode is not particularly limited, and the solid-liquid separation means known to those skilled in the art, such as filtration or centrifugal separation, can be adopted; in one embodiment, the filter is squeezed with a 200 mesh screen. And after the solid-liquid separation, obtaining filtrate and filter residue, and taking the filtrate for subsequent extraction.
In the present invention, it is preferable to cool the solid-liquid separation before the solid-liquid separation; in one embodiment, cooling to below 50 ℃ is followed by solid-liquid separation.
In the present invention, after the solid-liquid separation to obtain the filtrate, it is preferable to perform a centrifugal treatment on the filtrate, and to take the supernatant for subsequent extraction.
In the step c2), the mass ratio of the propylene glycol to the initial tobacco stems is preferably (80-120) to 100. The mixing and concentrating mode is not particularly limited, and the concentration means well known to those skilled in the art is adopted, so that the propylene glycol is fully fused with the filtrate through concentration; in one embodiment, the concentration is carried out by heating at 90-100 ℃ for 15-25 min. In the invention, the mass ratio of the volume of the concentrated liquid to the initial tobacco stems is preferably (180-250) mL: 100 g. After the concentration, an extract is obtained.
More preferably, the step c1) specifically includes:
c1-1) mixing the reactant with ethanol, heating, and carrying out solid-liquid separation to obtain a first filtrate and filter residue;
c1-2) mixing and heating the filter residue and ethanol, and carrying out solid-liquid separation to obtain a second filtrate;
c1-3) combining the first filtrate with the second filtrate to obtain a filtrate.
The parameter conditions and the like in step c1-1) are the same as those in the above technical solution, and are not described herein again. And carrying out solid-liquid separation to obtain a first filtrate and filter residue.
In the step c1-2), the mass percentage concentration of the ethanol is preferably 30-50%. The mass ratio of the ethanol to the initial tobacco stems is preferably (350-45) to 100. The mixing and heating temperature is preferably 85-95 ℃; the mixing and heating time is preferably 0.8-1.2 h. After the mixing and heating, solid-liquid separation is performed. The solid-liquid separation mode is not particularly limited, and the solid-liquid separation means known to those skilled in the art, such as filtration or centrifugal separation, can be adopted; in one embodiment, the filter is squeezed with a 200 mesh screen. After the solid-liquid separation, a second filtrate is obtained. In the present invention, it is preferable to cool the solid-liquid separation before the solid-liquid separation; in one embodiment, cooling to below 50 ℃ is followed by solid-liquid separation. After the first filtrate and the second filtrate are obtained, the first filtrate and the second filtrate are combined to obtain filtrate for subsequent extraction. In the present invention, it is preferable that the filtrate is centrifuged, and the supernatant is taken and subjected to subsequent extraction to obtain an extract.
According to the invention, after the extracting solution is obtained, the extracting solution reacts with the compound additive to obtain the tobacco stem extract.
In the invention, the compound additives comprise cellulase, xylose, fructose and vitamin C. The composite additive is adopted to react with the extracting solution, so that the aroma components of the tobacco baking flavor can be effectively increased, and the smoking quality of tobacco products is remarkably improved. In the composite additive, the mass ratio of the cellulase, the xylose, the fructose and the vitamin C is preferably (0.18-0.22): (0.28-0.32): (0.04-0.06): (0.18-0.22). In the invention, the mass ratio of the composite additive to the tobacco stems is preferably (0.68-0.82) to 100. More preferably, the mass ratio of the cellulase to the tobacco stems is (0.18-0.22) to 100; the mass ratio of the xylose to the tobacco stems is (0.28-0.32) to 100; the mass ratio of the fructose to the tobacco stems is (0.04-0.06) to 100; the mass ratio of the vitamin C to the tobacco stems is (0.18-0.22) to 100.
In the invention, the reaction temperature is preferably 90-100 ℃; the reaction time is preferably 2.5-3.5 h. After the reaction, a tobacco extract is produced.
In the present invention, it is preferable to further perform solid-liquid separation after the reaction, and the obtained separated liquid is a tobacco extract. The solid-liquid separation method is not particularly limited, and the solid-liquid separation means known to those skilled in the art, such as filtration or centrifugal separation, can be adopted. In the present invention, it is preferable to cool the solid-liquid separation before the solid-liquid separation; in one embodiment, cooling to below 50 ℃ is followed by solid-liquid separation.
The preparation method provided by the invention can effectively remove negative taste substances in the tobacco stems, which influence the taste of smoking, can promote substance conversion, increase a large amount of fragrant substances with tobacco aroma, and greatly improve the smoking quality of tobacco products. Meanwhile, the preparation method is simple and feasible, simple in equipment, mild in condition and convenient for large-scale production and application; the invention does not relate to the recovery of toxic solvent, and is more environment-friendly.
The invention also provides the tobacco stem extract prepared by the preparation method in the technical scheme. The tobacco extract greatly reduces negative taste absorbing substances which influence the taste of smoking, has a large amount of fragrant substances with tobacco roasting fragrance, and can remarkably improve the smoking quality of tobacco products.
The invention also provides a tobacco product which comprises the tobacco stem extract in the technical scheme. The tobacco stem extract is added into the tobacco product, so that a large amount of negative taste absorbing substances can be avoided, the tobacco product has roasted aroma flavor, and the smoking quality of the tobacco product is obviously improved. In the invention, the addition amount of the tobacco stem extract in the tobacco product is preferably 0.005-0.1 wt%. The type of the tobacco product is not particularly limited in the present invention, and the tobacco product is known to those skilled in the art, such as a cigarette, a cigar, a tobacco sheet, and the like.
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
Example 1
1.1 preparation of samples
Adding 100g of tobacco stem powder and 750g of purified water into a 1000mL round-bottom flask, and heating in a water bath at 50 ℃ for 30min to obtain tobacco stem liquid; adding 0.1g of cellulase, 0.2g of pectinase, 0.1g of xylanase, 0.22g of protease, 0.2g of amylase and 0.1g of glucoamylase into 30g of purified water, uniformly mixing in a beaker, activating at 25 ℃ for 20min, transferring into the round-bottom flask, cleaning the beaker with the purified water twice, 10g of purified water each time, transferring the cleaning solution into the round-bottom flask together, and reacting for 6.5h in a water bath at 50 ℃. After reaction, 429g of 95% ethanol is added into a round-bottom flask, and then the round-bottom flask is placed in a water bath at 90 ℃ for reflux extraction for 1 hour; after the reaction is finished, cooling the flask to below 50 ℃, squeezing and filtering by using a 200-mesh net, reserving filtrate for later use, and returning filter residues to an original bottle; adding 400g of 40% ethanol into a filter residue bottle, performing reflux extraction in a water bath at 90 ℃ for 1h, cooling to below 50 ℃, and performing squeezing filtration by using a 200-mesh net to obtain a filtrate. Mixing the two filtrates, centrifuging, and collecting supernatant; adding 100g propylene glycol into the supernatant, mixing well in 500mL round-bottom flask, heating at 50 deg.C to concentrate to 200mL, and heating in boiling water bath for 20min to obtain extractive solution. Then, 0.2g of cellulase, 0.3g of xylose, 0.05g of fructose and 0.2g of vitamin C are added, the mixture is refluxed for 3 hours in boiling water bath, and then cooled to below 50 ℃, and the filtrate is filtered, namely the tobacco stem extract (marked as S1).
Preparation of control:
the solvent extraction method comprises the following steps: connecting one end of a simultaneous distillation and extraction device with a 1000mL round-bottom flask, filling 100g of tobacco stem powder and 500mL of purified water in the flask, and heating at 100 ℃ by using an electric furnace with controllable voltage; the other end of the apparatus was connected to a 100mL flask containing 40mL of methylene chloride, and the flask was heated in a water bath at 60 ℃. After the above simultaneous distillation and extraction treatment was carried out for 2 hours, 6g of anhydrous sodium sulfate was added to the dichloromethane extract, and the mixture was dried overnight to obtain a tobacco stem extract control (marked as D-1).
1.2 detection of samples
(1) According to the national standards GB/T10742 and 191989, YC/T216 and 2013 and YC/T166 and 2003, the negative taste components such as pectin, starch, protein and the like in the tobacco stem extract S1 are measured, and the result shows that the negative taste components are not detected, so that the preparation method provided by the invention is proved to eliminate a large amount of negative adsorption substances which influence the taste of the tobacco stem.
(2) The aroma components of the tobacco stem extract S1 and the control D-1 were tested by GC-MS gas chromatography.
GC conditions were as follows: a chromatographic column: INNOWAX, 60 m.times.0.25 mm.times.0.25 μm; carrier gas: he; flow rate of carrier gas: 1 mL/min; sample introduction mode: no flow diversion; sample inlet temperature: 250 ℃; temperature rising procedure: maintaining at 40 deg.C for 20min, increasing to 160 deg.C at 2 deg.C/min, maintaining for 20min, and increasing to 230 deg.C at 2 deg.C/min for 2 min;
MS conditions: an ion source: an EI source; ion source temperature: 230 ℃; electron energy: 70 eV; scanning mode: and (4) full scanning.
The results show that the obtained tobacco stem extract S1 has a large amount of new aroma substances added compared with the control D-1, and the specific substances and contents are increased as shown in Table 1.
TABLE 1 increased flavor content and flavor content of cabo extract S1
As can be seen from the test results in Table 1, by the preparation method, a large amount of flavor components are added, the aroma of the tobacco products can be enriched, and the smoking quality is remarkably improved.
Example 2
1.1 preparation of samples
Adding 100g of tobacco stem powder and 700g of purified water into a 1000mL round-bottom flask, and heating in a water bath at 50 ℃ for 30min to obtain tobacco stem liquid; adding 0.08g of cellulase, 0.18g of pectinase, 0.08g of xylanase, 0.20g of protease, 0.18g of amylase and 0.08g of glucoamylase into 30g of purified water, uniformly mixing in a beaker, activating at 25 ℃ for 20min, transferring into the round-bottom flask, cleaning the beaker with the purified water twice, 10g of purified water each time, transferring the cleaning solution into the round-bottom flask together, and reacting for 6.5h in a water bath at 50 ℃. After reaction, 429g of 95% ethanol is added into a round-bottom flask, and then the round-bottom flask is placed in a water bath at 90 ℃ for reflux extraction for 1 hour; after the reaction is finished, cooling the flask to below 50 ℃, squeezing and filtering by using a 200-mesh net, reserving filtrate for later use, and returning filter residues to an original bottle; adding 400g of 40% ethanol into a filter residue bottle, performing reflux extraction in a water bath at 90 ℃ for 1h, cooling to below 50 ℃, and performing squeezing filtration by using a 200-mesh net to obtain a filtrate. Mixing the two filtrates, centrifuging, and collecting supernatant; adding 100g propylene glycol into the supernatant, mixing well in 500mL round-bottom flask, heating at 50 deg.C to concentrate to 200mL, and heating in boiling water bath for 20min to obtain extractive solution. Then, 0.18g of cellulase, 0.28g of xylose, 0.04g of fructose and 0.18g of vitamin C are added, the mixture is refluxed for 3 hours in boiling water bath, and then cooled to below 50 ℃, and the filtrate is filtered, namely the tobacco stem extract (marked as S2).
1.2 detection of samples
(1) Negative taste components such as pectin, starch, protein and the like in the tobacco stem extract S2 were measured according to the test method of example 1, and the results showed no detection.
(2) The aroma components of the resulting tobacco stem extract S2 were tested according to the test method of example 1 and compared with the control D-1, and the results are shown in Table 2.
TABLE 2 increased flavor content and flavor content of cabo extract S2
Example 3
1.1 preparation of samples
Adding 100g of tobacco stem powder and 800g of purified water into a 1000mL round-bottom flask, and heating in a water bath at 50 ℃ for 30min to obtain tobacco stem liquid; adding 0.12g of cellulase, 0.22g of pectinase, 0.12g of xylanase, 0.24g of protease, 0.22g of amylase and 0.12g of glucoamylase into 30g of purified water, uniformly mixing in a beaker, activating at 25 ℃ for 20min, transferring into the round-bottom flask, cleaning the beaker with the purified water twice, 10g of purified water each time, transferring the cleaning solution into the round-bottom flask together, and reacting for 6.5h in a water bath at 50 ℃. After reaction, 429g of 95% ethanol is added into a round-bottom flask, and then the round-bottom flask is placed in a water bath at 90 ℃ for reflux extraction for 1 hour; after the reaction is finished, cooling the flask to below 50 ℃, squeezing and filtering by using a 200-mesh net, reserving filtrate for later use, and returning filter residues to an original bottle; adding 400g of 40% ethanol into a filter residue bottle, performing reflux extraction in a water bath at 90 ℃ for 1h, cooling to below 50 ℃, and performing squeezing filtration by using a 200-mesh net to obtain a filtrate. Mixing the two filtrates, centrifuging, and collecting supernatant; adding 100g propylene glycol into the supernatant, mixing well in 500mL round-bottom flask, heating at 50 deg.C to concentrate to 200mL, and heating in boiling water bath for 20min to obtain extractive solution. Then, 0.22g of cellulase, 0.32g of xylose, 0.06g of fructose and 0.22g of vitamin C are added, the mixture is refluxed for 3 hours in boiling water bath, and then cooled to below 50 ℃, and the filtrate is filtered, namely the tobacco stem extract (marked as S3).
1.2 detection of samples
(1) Negative taste components such as pectin, starch, protein and the like in the tobacco stem extract S3 were measured according to the test method of example 1, and the results showed no detection.
(2) The aroma components of the resulting tobacco stem extract S3 were tested according to the test method of example 1 and compared with the control D-1, and the results are shown in Table 3.
TABLE 3 increased flavor content and flavor content of cabo extract S3
According to the test results of the examples 1-3, the preparation method disclosed by the invention can be used for eliminating a large amount of negative odor absorbing substances in the tobacco stems; meanwhile, by the preparation method, a large number of components with natural faint scent and baking aroma are added, and the aroma components can enrich the aroma of the tobacco products and greatly improve the smoking quality. In addition, compared with the existing chemical extraction mode, the preparation method provided by the invention has the advantages that toxic and harmful reagents are not needed in the preparation process, the environmental pollution is reduced, the cost is reduced, the preparation process is simple and feasible, the condition is mild, and the large-scale production is facilitated.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. The preparation method of the tobacco stem extract is characterized by comprising the following steps:
a) mixing and heating tobacco stems and water to obtain tobacco stem liquid;
the mass ratio of the tobacco stems to the water is 100: 650-900; the mixing and heating temperature is 45-55 ℃, and the time is 25-35 min;
mixing and activating the complex enzyme and water to obtain an enzyme dispersion liquid;
the complex enzyme is cellulase, pectinase, xylanase, protease, amylase and glucoamylase;
the mass ratio of the complex enzyme to the tobacco stems is (0.80-1.04) to 100;
b) mixing the tobacco stalk liquid and an enzyme dispersion liquid, and heating for reaction to obtain a reactant;
c1-1) mixing the reactant with ethanol, heating, and carrying out solid-liquid separation to obtain a first filtrate and filter residue;
c1-2) mixing and heating the filter residue and ethanol, and carrying out solid-liquid separation to obtain a second filtrate;
c1-3) combining the first filtrate and the second filtrate to obtain a filtrate;
c2) mixing the filtrate with propylene glycol, and concentrating to obtain an extracting solution;
d) reacting the extracting solution with a compound additive to obtain a tobacco stem extract;
the compound additive comprises cellulase, xylose, fructose and vitamin C;
in the compound enzyme, the mass ratio of cellulase, pectinase, xylanase, protease, amylase and glucoamylase is (0.08-0.12): (0.18-0.22): (0.08-0.12): (0.20-0.24): (0.18-0.22): (0.08-0.12);
in the composite additive, the mass ratio of cellulase to xylose to fructose to vitamin C is (0.18-0.22) to (0.28-0.32) to (0.04-0.06) to (0.18-0.22);
the mass ratio of the composite additive to the tobacco stems is (0.68-0.82) to 100.
2. The preparation method according to claim 1, wherein in the step b), the heating reaction is carried out at a temperature of 45-55 ℃ for 6-7 hours.
3. The preparation method according to claim 1, wherein the reaction temperature in step d) is 90-100 ℃ and the reaction time is 2.5-3.5 h.
4. The preparation method of claim 1, wherein in the step a), when the complex enzyme and water are mixed and activated, the mass ratio of the complex enzyme to the water is (0.80-1.04) to (30-50); the temperature of mixing activation is 20-30 ℃, and the time is 15-25 min.
5. A tobacco stem extract obtained by the method of any one of claims 1 to 4.
6. A tobacco product comprising the stem extract of claim 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810645182.6A CN109007955B (en) | 2018-06-21 | 2018-06-21 | Tobacco stem extract, preparation method thereof and tobacco product |
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| CN112075657B (en) * | 2020-08-27 | 2022-09-16 | 重庆中烟工业有限责任公司 | Preparation method and application of tobacco stem extract |
| CN115137091A (en) * | 2022-07-11 | 2022-10-04 | 湖北中烟工业有限责任公司 | Method for extracting waste tobacco stems of cigars |
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