CN115137091A - Method for extracting waste tobacco stems of cigars - Google Patents
Method for extracting waste tobacco stems of cigars Download PDFInfo
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- CN115137091A CN115137091A CN202210810199.9A CN202210810199A CN115137091A CN 115137091 A CN115137091 A CN 115137091A CN 202210810199 A CN202210810199 A CN 202210810199A CN 115137091 A CN115137091 A CN 115137091A
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Images
Classifications
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
-
- 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
-
- 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
-
- 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
- A24B15/26—Use of organic solvents for extraction
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
The invention discloses a method for extracting waste tobacco stems of cigars, which comprises the steps of preliminarily extracting the tobacco stems by an enzymolysis method, simultaneously destroying intercellular layers and cell walls among cells, further destroying inner cell layers, simulating the environment that oral drugs are transported and absorbed through gastrointestinal tracts, and carrying out acid-base digestion treatment on enzymolysis liquid, so that active ingredients in the tobacco stems are leached out very favorably, then distilling and extracting active substances in the tobacco stems by adopting a distillation extraction technology, finally filtering and precipitating alcohol, removing negative-acting ingredients such as protein, pectin and the like in an extract, and greatly improving the yield of the active ingredients such as nicotine, polysaccharide and the like.
Description
Technical Field
The invention relates to the technical field of tobacco stem extraction, in particular to a method for extracting waste tobacco stems of cigars.
Background
Cigars are a unique tobacco product, and traditionally cigars are smoking cigarettes that are all manually wrapped with tobacco leaves. The cigar has the characteristics of rich fragrance, unique cultural charm and the like, is accepted by a plurality of tobacco consumers in recent years, and the development of the domestic cigar enters a rapid rising stage after the restriction factors such as production process, equipment and the like are gradually solved. With the improvement of economic level and the improvement of living standard of people, the demand of cigars in China is continuously increased. However, in the production process of cigar tobacco, a large amount of waste tobacco stems are generated, and the waste tobacco stems are generally thrown away as waste. Therefore, the method not only pollutes the environment, but also causes a great deal of resource waste.
The tobacco stems are coarse and hard stem veins of tobacco leaves, are byproducts of the cigarette industry, account for about 25% -30% of the total weight of the tobacco leaves, millions of tons of tobacco stems are generated in China every year, and the application of the tobacco stems has more ways, but due to technical limitation, the utilization rate of the tobacco stems is only 40% so far, dozens of thousands of tons of tobacco stems are still discarded every year, and the tobacco stems cannot be used in cigarette production. The tobacco stem waste generated in the production process of the cigar tobacco leaves contains toxic compounds such as nicotine and the like, and cannot be treated together with common garbage, so that the improper treatment of the tobacco stem waste can cause environmental pollution and also can cause great waste of resources. On the other hand, the chemical composition of the tobacco stems is very similar to that of tobacco leaves, the tobacco essential oil prepared from the tobacco stems has various key aroma substances in the tobacco, and the tobacco essential oil can transmit the original tobacco aroma and cover the miscellaneous gas and the woody smell of the tobacco sheets when being added to the tobacco sheets or the tobacco leaves, and the original tobacco aroma cannot be replaced by other tobacco essences added with single components. Therefore, if the waste tobacco stems can be fully utilized in the cigarette making process, the cost for treating waste can be reduced, a new way for high-value utilization of the tobacco stems can be opened up, and the method has very important significance.
For example, the application number is [ CN202110545436.9 ] a method for preparing cigar flavor from cigar waste, flavor and application thereof, the cigar waste is extracted by a solvent method to obtain cigar extract, and the cigar tobacco extract is concentrated under reduced pressure; precipitating with ethanol, freezing to remove wax, filtering, collecting filtrate to obtain cigar flavor, and concentrating under reduced pressure to obtain dry matter. The cigar flavor prepared by the invention is sprayed on the domestic single-material cigar tobacco leaves, and rolled into cigar finished products, and through sensory evaluation, the cigar flavor can increase the fragrance and the nut fragrance of sun-cured tobaccos, increase the natural sweetness of tobaccos, enrich the fragrance, improve the sense of hierarchy, and enable the smoke to be fine, mellow and fine, thereby effectively improving the problems of hardness and heavy miscellaneous gas of the domestic cigar smoke. The method also improves the comprehensive utilization rate of high-quality cigar raw materials, reduces the cost of the raw materials, and can be applied to the flavoring of cigarettes, cigar tobacco products and novel tobacco products.
In the process, as the waste tobacco stems of the cigar tobacco leaves have more impurities and some toxic and harmful chemical substances, the effective substances in the tobacco stems are not easy to dissolve in the solvent, the extraction rate is low by adopting a conventional solvent extraction method, and the prepared spice has poor effect.
Disclosure of Invention
In order to solve the problems, the invention provides an extraction method of the waste tobacco stems of the cigars, which is used for extracting the tobacco stems of the cigars, and the extract can be added into tobacco leaves to enhance the smoking experience of the tobacco leaves, achieve the purpose of recycling wastes, protect the environment and create economic value.
In order to achieve the purpose, the invention is realized by the following technical scheme: the invention provides a method for extracting waste tobacco stems of cigars, which comprises the following steps:
s1, collecting waste tobacco stems, removing impurities, drying, grinding the tobacco stems into powder by using a plant sample grinder, and sieving the powder by using a 40-mesh sieve for later use;
preferably, the tobacco stems are dried in a 40 ℃ forced air drying oven for 12 hours in S1.
The method comprises the steps of washing the collected waste tobacco stems of the cigars, and then drying the tobacco stems in a 40 ℃ forced air drying oven for 12 hours, so that impurities and sewage can be effectively removed. And then grinding the tobacco stems into powder by a plant sample grinder, and sieving the powder by a 40-mesh sieve to obtain the treated waste tobacco stem powder, so that the dissolution and pretreatment of the tobacco stems in the later period are facilitated.
S2, dissolving the tobacco stalk powder in the S1 in water, adding the combined enzyme for enzymolysis for 40-50min, and filtering to obtain an enzymolysis solution;
preferably, the combined enzyme in S2 comprises pectinase, cellulase and protease at a mass ratio of 1:1:1.
preferably, the mass ratio of the tobacco stem powder, the water and the combined enzyme in the S2 is 40:400: (0.4-2).
In order to separate out effective substances in the tobacco stems, the tobacco stems are dissolved in water, then the combined enzyme is added to carry out enzymolysis treatment on the tobacco stem powder, and the cell walls of the tobacco stems can be damaged by the combined enzyme, so that the effective substances in the tobacco stems are separated out.
The enzymolysis method utilizes the high specificity of enzyme, selects proper enzyme to degrade the cell wall of the raw material, makes the intracellular components enter the extracting solvent more easily, and simultaneously can protect the effective components from being damaged due to the mild reaction condition of enzymolysis.
However, the extraction effect achieved by only destroying the cell wall by enzymolysis is not complete, so the invention carries out acid-base treatment on the enzymolysis liquid.
S3, adding 10-15% of sodium hydroxide aqueous solution into the enzymatic hydrolysate in the S2, uniformly stirring, standing for 2-3 hours, adding 0.5-3% of dilute sulfuric acid solution, heating, refluxing and extracting for 2 hours, filtering the solution, and concentrating under reduced pressure to obtain a concentrated solution;
preferably, the mass ratio of the enzymolysis liquid in the S3, the sodium hydroxide aqueous solution and the dilute sulfuric acid solution is (4-5): 1: (15-20).
According to the invention, the enzymolysis liquid is subjected to alkali treatment and then acid treatment, and the residual protease in the enzymolysis liquid is combined, so that the environment that oral drugs are transported and absorbed through gastrointestinal tracts can be simulated, and the tobacco stems are subjected to digestion-like treatment, thereby being very beneficial to leaching of active ingredients in the tobacco stems.
The effective substances in the tobacco stems after the acid and alkali treatment can be fully dissolved out, and then the invention needs to extract the effective substances.
S4, distilling and extracting the concentrated solution obtained in the step S3 to obtain distillate;
preferably, the extract solution distilled and extracted in S4 is an ethanol solution with a mass concentration of 70%.
Preferably, the mass ratio of the concentrated solution to the extracting solution in the S4 is 1:10.
preferably, the extraction temperature in the S4 is 70-72 ℃, and the extraction time is 1h.
The distillation extraction is carried out by utilizing the difference of molecular free path of each substance in the mixture. The molecules are heated and overflow from the liquid surface of the material, because the mean free path of the light molecules is greater than that of the heavy molecules, when the distance between the condensing surface and the heating surface is smaller than that of the light molecules and greater than that of the heavy molecules, the light molecules can reach the condensing surface to be collected and continuously escape from the surface of the material, and the heavy molecules cannot reach the condensing surface due to the smaller mean free path and return to the heating surface, so that the light and heavy components are separated.
Because the components of the fractions at different temperatures are obviously different, the active ingredients in the tobacco stems can be selectively enriched by distillation and extraction, the fractions at 70-72 ℃ are collected, and the components of the fractions are mostly active substances in the tobacco stems, so that other ineffective impurities in the extracting solution can be removed, and the active substances in the tobacco stems can be selectively extracted.
The distillation extraction in the invention is similar to the effect of simulated smoking of the extract in the process of smoking tobacco leaves by consumers after the extract is added into the tobacco leaves at the later stage, when the combustion temperature of the tobacco reaches 70 ℃, namely the distillation temperature of the invention reaches 70 ℃, the effective components in the extract can be fully volatilized at the moment, and enter the oral cavity of a human body along with the smoke, therefore, the distillation extraction in the invention is equivalent to the pre-screening of the effective substances. Thus, when the extract prepared by the invention is added into tobacco leaves for smoking at a later stage, the smoking taste is pure, and the residual pungent smell in the tobacco stems before distillation is removed. Therefore, the distillation extraction of the invention can refine and purify the tobacco extract.
And S5, filtering the distillate in the step S4 by using a 0.8-micron filter membrane to obtain a filtrate, adding 70% ethanol by mass concentration to carry out ethanol precipitation, standing the solution obtained by ethanol precipitation in a refrigerator overnight, filtering and concentrating the next day to obtain a crude extract, and finally adding propylene glycol to obtain the waste tobacco stem extract.
Preferably, the mass ratio of the filtrate to the ethanol in the S5 is 1:5.
preferably, the mass ratio of the crude extract in the S5 to the propylene glycol is 100:15.
and (3) carrying out alcohol precipitation separation on the distillate collected after extraction, and finally collecting the concentrate, namely the waste tobacco stem extract.
According to the tobacco stem extractive and the preparation method thereof, the biological enzymolysis method, the acid-base pretreatment and the distillation extraction are used cooperatively, so that volatile effective substances in the tobacco stems can be fully extracted, the enzyme method is adopted for assistance, the yield of the effective substances is obviously improved, the contents of reducing sugar and nicotine in the tobacco stem extractive are obviously increased after the acid-base pretreatment, the yield of Maillard reaction products is obviously increased, the content of the effective substances in the tobacco stem extractive is greatly improved, and the smoking feeling of the tobacco leaves can be obviously improved when the tobacco stem extractive is added into the tobacco leaves for smoking in the later period.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the method for extracting the waste tobacco stems of the cigars, provided by the invention, the tobacco stems are preliminarily extracted through an enzymolysis method, so that intercellular layers and cell walls among cells can be simultaneously damaged, then inner layers of the cells are damaged, then the environment that oral medicines are transported and absorbed through gastrointestinal tracts is simulated, and acid-base digestion treatment is carried out on enzymolysis liquid, so that active ingredients in the tobacco stems are very favorably leached out, then the distillation extraction technology is adopted, effective substances in the tobacco stems are distilled and extracted, finally, filtration and alcohol precipitation are carried out, negative-acting ingredients such as protein, pectin and the like in the extract are removed, and the yield of the active ingredients such as nicotine, polysaccharide and the like is greatly improved.
2. The method for extracting the waste tobacco stems of the cigars has the advantages of short extraction time and low temperature, can fully extract active ingredients in the tobacco stems, adjusts the pH value in the extraction process, and can enable the properties of the tobacco stem extracts to be more stable through low-temperature alcohol precipitation and other modes.
Drawings
Fig. 1 is a preparation flow chart of a method for extracting waste tobacco stems of cigars in the embodiment of the invention.
Detailed Description
In order to more clearly illustrate the embodiments of the present invention and the technical solutions in the prior art, the following will describe the specific embodiments of the present invention with reference to the accompanying drawings.
It is obvious that the drawings in the following description are only some examples of the invention, and it is obvious to a person skilled in the art that other drawings and other embodiments can be obtained from these drawings without inventive effort, and the invention is not limited to this example.
The specific embodiment of the invention is as follows:
example 1
A method for extracting waste tobacco stems of cigars comprises the following steps:
s1, collecting waste tobacco stems, removing impurities, drying the tobacco stems in a forced air drying box at 40 ℃ for 11 hours, grinding the tobacco stems into powder by using a plant sample grinder, and sieving the powder by using a 40-mesh sieve for later use;
s2, 300g of tobacco stem powder in the S1 is taken and dissolved in 3000g of water, 3g of combined enzyme is added for enzymolysis for 40min, and enzymolysis liquid is obtained through filtration, wherein the combined enzyme comprises pectinase, cellulase and protease in a mass ratio of 1:1:1;
and S3, adding a sodium hydroxide aqueous solution with the mass concentration of 10% into the enzymolysis liquid in the S2, uniformly stirring, standing for 2 hours, adding a dilute sulfuric acid solution with the mass concentration of 0.5%, heating, refluxing and extracting for 2 hours, filtering the solution, and concentrating under reduced pressure to obtain a concentrated solution, wherein the mass ratio of the enzymolysis liquid to the sodium hydroxide aqueous solution to the dilute sulfuric acid solution is 4:1:15;
and S4, distilling and extracting the concentrated solution in the step S3 to obtain distillate, wherein the distilled and extracted extracting solution is an ethanol solution with the mass concentration of 70%, and the mass ratio of the concentrated solution to the extracting solution is 1:10, wherein the temperature of distillation extraction is 70 ℃, and the extraction time is 1h;
s5, filtering the distillate in the step S4 with a 0.8-micron filter membrane to obtain a filtrate, adding 70% ethanol in mass concentration for ethanol precipitation, standing the solution obtained by ethanol precipitation in a refrigerator overnight, filtering and concentrating the next day to obtain 200g of crude extract, and finally adding 30g of propylene glycol to obtain the waste tobacco stem extract, wherein the mass ratio of the filtrate to the ethanol is 1:5.
example 2
A method for extracting waste tobacco stems of cigars comprises the following steps:
s1, collecting waste tobacco stems, removing impurities, drying the tobacco stems in a 41-DEG C forced air drying oven for 11 hours, grinding the tobacco stems into powder by using a plant sample grinder, and sieving the powder by using a 40-mesh sieve for later use;
s2, 300g of tobacco stem powder in the S1 is taken and dissolved in 3000g of water, 3g of combined enzyme is added for enzymolysis for 42min, and enzymolysis liquid is obtained through filtration, wherein the combined enzyme comprises pectinase, cellulase and protease in a mass ratio of 1:1:1;
and S3, adding 11% of sodium hydroxide aqueous solution into the enzymatic hydrolysate in the step S2, uniformly stirring, standing for 2 hours, adding 1% of dilute sulfuric acid solution, heating, refluxing and extracting for 2 hours, filtering the solution, and concentrating under reduced pressure to obtain a concentrated solution, wherein the mass ratio of the enzymatic hydrolysate to the sodium hydroxide aqueous solution to the dilute sulfuric acid solution is 4:1:16;
and S4, distilling and extracting the concentrated solution in the step S3 to obtain distillate, wherein the distilled and extracted extracting solution is an ethanol solution with the mass concentration of 70%, and the mass ratio of the concentrated solution to the extracting solution is 1:10, wherein the temperature of distillation extraction is 71 ℃, and the extraction time is 1h;
s5, filtering the distillate in the step S4 with a 0.8-micron filter membrane to obtain a filtrate, adding 70% ethanol in mass concentration for ethanol precipitation, standing the solution obtained by ethanol precipitation in a refrigerator overnight, filtering and concentrating the next day to obtain 200g of crude extract, and finally adding 30g of propylene glycol to obtain the waste tobacco stem extract, wherein the mass ratio of the filtrate to the ethanol is 1:5.
example 3
A method for extracting waste tobacco stems of cigars comprises the following steps:
s1, collecting waste tobacco stems, removing impurities, drying the tobacco stems in a forced air drying box at 41 ℃ for 11.5 hours, grinding the tobacco stems into powder by using a plant sample grinder, and sieving the powder by using a 40-mesh sieve for later use;
s2, 300g of tobacco stem powder in the S1 is taken and dissolved in 3000g of water, 3g of combined enzyme is added for enzymolysis for 44min, and enzymolysis liquid is obtained through filtration, wherein the combined enzyme comprises pectinase, cellulase and protease in a mass ratio of 1:1:1;
and S3, adding the enzymolysis liquid in the S2 into a sodium hydroxide aqueous solution with the mass concentration of 12%, uniformly stirring, standing for 2.5 hours, adding a dilute sulfuric acid solution with the mass concentration of 1.5%, heating, refluxing and extracting for 2 hours, filtering the solution, and concentrating under reduced pressure to obtain a concentrated solution, wherein the mass ratio of the enzymolysis liquid to the sodium hydroxide aqueous solution to the dilute sulfuric acid solution is 4:1:17;
s4, distilling and extracting the concentrated solution obtained in the step S3 to obtain a distillate, wherein the distilled and extracted extracting solution is an ethanol solution with the mass concentration of 70%, and the mass ratio of the concentrated solution to the extracting solution is 1:10, wherein the temperature of distillation extraction is 71 ℃, and the extraction time is 1h;
s5, filtering the distillate in the step S4 by using a 0.8-micron filter membrane to obtain a filtrate, adding 70% ethanol in mass concentration for ethanol precipitation, standing the solution obtained by the ethanol precipitation in a refrigerator overnight, filtering and concentrating the solution the next day to obtain 200g of crude extract, and finally adding 30g of propylene glycol to obtain the waste tobacco stem extract, wherein the mass ratio of the filtrate to the ethanol is 1:5.
example 4
A method for extracting waste tobacco stems of cigars comprises the following steps:
s1, collecting waste tobacco stems, removing impurities, drying the tobacco stems in a 42-DEG C forced air drying oven for 12 hours, grinding the tobacco stems into powder by using a plant sample grinder, and sieving the powder by using a 40-mesh sieve for later use;
s2, dissolving 300g of tobacco stem powder in the S1 in 3000g of water, adding 3g of combined enzyme for enzymolysis for 48min, and filtering to obtain enzymatic hydrolysate, wherein the combined enzyme comprises pectinase, cellulase and protease in a mass ratio of 1:1:1;
and S3, adding the enzymolysis liquid in the S2 into a sodium hydroxide aqueous solution with the mass concentration of 14%, uniformly stirring, standing for 3 hours, adding a dilute sulfuric acid solution with the mass concentration of 2%, heating, refluxing and extracting for 2 hours, filtering the solution, and concentrating under reduced pressure to obtain a concentrated solution, wherein the mass ratio of the enzymolysis liquid to the sodium hydroxide aqueous solution to the dilute sulfuric acid solution is 5:1:18;
and S4, distilling and extracting the concentrated solution in the step S3 to obtain distillate, wherein the distilled and extracted extracting solution is an ethanol solution with the mass concentration of 70%, and the mass ratio of the concentrated solution to the extracting solution is 1:10, wherein the temperature of distillation extraction is 72 ℃, and the extraction time is 1h;
s5, filtering the distillate in the step S4 with a 0.8-micron filter membrane to obtain a filtrate, adding 70% ethanol in mass concentration for ethanol precipitation, standing the solution obtained by ethanol precipitation in a refrigerator overnight, filtering and concentrating the next day to obtain 200g of crude extract, and finally adding 30g of propylene glycol to obtain the waste tobacco stem extract, wherein the mass ratio of the filtrate to the ethanol is 1:5.
example 5
A method for extracting waste tobacco stems of cigars comprises the following steps:
s1, collecting waste tobacco stems, removing impurities, drying the tobacco stems in a 42-DEG C forced air drying oven for 12 hours, grinding the tobacco stems into powder by using a plant sample grinder, and sieving the powder by using a 40-mesh sieve for later use;
s2, 300g of tobacco stem powder in the S1 is taken and dissolved in 3000g of water, 3g of combined enzyme is added for enzymolysis for 50min, and enzymolysis liquid is obtained through filtration, wherein the combined enzyme comprises pectinase, cellulose and protease in a mass ratio of 1:1:1;
and S3, adding the enzymolysis liquid in the S2 into a sodium hydroxide aqueous solution with the mass concentration of 15%, uniformly stirring, standing for 3 hours, adding a dilute sulfuric acid solution with the mass concentration of 3%, heating, refluxing and extracting for 2 hours, filtering the solution, and concentrating under reduced pressure to obtain a concentrated solution, wherein the mass ratio of the enzymolysis liquid to the sodium hydroxide aqueous solution to the dilute sulfuric acid solution is 5:1:20;
and S4, distilling and extracting the concentrated solution in the step S3 to obtain distillate, wherein the distilled and extracted extracting solution is an ethanol solution with the mass concentration of 70%, and the mass ratio of the concentrated solution to the extracting solution is 1:10, wherein the temperature of distillation extraction is 72 ℃, and the extraction time is 1h;
s5, filtering the distillate in the step S4 with a 0.8-micron filter membrane to obtain a filtrate, adding 70% ethanol in mass concentration for ethanol precipitation, standing the solution obtained by ethanol precipitation in a refrigerator overnight, filtering and concentrating the next day to obtain 200g of crude extract, and finally adding 30g of propylene glycol to obtain the waste tobacco stem extract, wherein the mass ratio of the filtrate to the ethanol is 1:5.
comparative example 1
The difference between comparative example 1 and example 3 is that the enzymolysis was carried out without adding the enzyme combination in comparative example 1. The method comprises the following specific steps:
a method for extracting waste tobacco stems of cigars comprises the following steps:
s1, collecting waste tobacco stems, removing impurities, drying the tobacco stems in a forced air drying box at 41 ℃ for 11.5 hours, grinding the tobacco stems into powder by using a plant sample grinder, and sieving the powder by using a 40-mesh sieve for later use;
s2, dissolving 300g of tobacco stalk powder in the S1 in 3000g of water to obtain hydrolysate;
and S3, adding the hydrolysate in the S2 into a sodium hydroxide aqueous solution with the mass concentration of 12%, uniformly stirring, standing for 2.5 hours, adding a dilute sulfuric acid solution with the mass concentration of 1.5%, heating, refluxing and extracting for 2 hours, filtering the solution, and concentrating under reduced pressure to obtain a concentrated solution, wherein the mass ratio of the hydrolysate to the sodium hydroxide aqueous solution to the dilute sulfuric acid solution is 4:1:17;
s4, distilling and extracting the concentrated solution obtained in the step S3 to obtain a distillate, wherein the distilled and extracted extracting solution is an ethanol solution with the mass concentration of 70%, and the mass ratio of the concentrated solution to the extracting solution is 1:10, wherein the temperature of distillation extraction is 71 ℃, and the extraction time is 1h;
s5, filtering the distillate in the step S4 with a 0.8-micron filter membrane to obtain a filtrate, adding 70% ethanol in mass concentration for ethanol precipitation, standing the solution obtained by ethanol precipitation in a refrigerator overnight, filtering and concentrating the next day to obtain 200g of crude extract, and finally adding 30g of propylene glycol to obtain the waste tobacco stem extract, wherein the mass ratio of the filtrate to the ethanol is 1:5.
comparative example 2
The difference between the comparative example 2 and the example 3 is that the acid-base digestion treatment is carried out on the enzymolysis liquid in the comparative example 2 without simulating the environment that the oral medicine is transported and absorbed through the gastrointestinal tract. The method comprises the following specific steps:
a method for extracting waste tobacco stems of cigars comprises the following steps:
s1, collecting waste tobacco stems, removing impurities, drying the tobacco stems in a 41-DEG C forced air drying oven for 11.5 hours, grinding the tobacco stems into powder by using a plant sample grinder, and sieving the powder through a 40-mesh sieve for later use;
s2, 300g of tobacco stem powder in the S1 is taken and dissolved in 3000g of water, 3g of combined enzyme is added for enzymolysis for 44min, and enzymolysis liquid is obtained through filtration, wherein the combined enzyme comprises pectinase, cellulase and protease in a mass ratio of 1:1:1;
and S3, distilling and extracting the enzymatic hydrolysate in the step S2 to obtain a distillate, wherein the distilled and extracted extracting solution is an ethanol solution with the mass concentration of 70%, and the mass ratio of the concentrated solution to the extracting solution is 1:10, wherein the temperature of distillation extraction is 71 ℃, and the extraction time is 1h;
s4, filtering the distillate in the step S3 with a 0.8-micron filter membrane to obtain a filtrate, adding 70% ethanol in mass concentration for ethanol precipitation, standing the solution obtained by ethanol precipitation in a refrigerator overnight, filtering and concentrating the next day to obtain 200g of crude extract, and finally adding 30g of propylene glycol to obtain the waste tobacco stem extract, wherein the mass ratio of the filtrate to the ethanol is 1:5.
comparative example 3
Comparative example 3 differs from example 3 in that no distillation extraction was performed in comparative example 3. The method comprises the following specific steps:
a method for extracting waste tobacco stems of cigars comprises the following steps:
s1, collecting waste tobacco stems, removing impurities, drying the tobacco stems in a 41-DEG C forced air drying oven for 11.5 hours, grinding the tobacco stems into powder by using a plant sample grinder, and sieving the powder through a 40-mesh sieve for later use;
s2, 300g of tobacco stem powder in the S1 is taken and dissolved in 3000g of water, 3g of combined enzyme is added for enzymolysis for 44min, and enzymolysis liquid is obtained through filtration, wherein the combined enzyme comprises pectinase, cellulase and protease in a mass ratio of 1:1:1;
and S3, adding the enzymolysis liquid in the S2 into a sodium hydroxide aqueous solution with the mass concentration of 12%, uniformly stirring, standing for 2.5 hours, adding a dilute sulfuric acid solution with the mass concentration of 1.5%, heating, refluxing and extracting for 2 hours, filtering the solution, and concentrating under reduced pressure to obtain a concentrated solution, wherein the mass ratio of the enzymolysis liquid to the sodium hydroxide aqueous solution to the dilute sulfuric acid solution is 4:1:17;
s4, filtering the concentrated solution obtained in the step S3 by using a 0.8-micron filter membrane to obtain a filtrate, adding 70% ethanol by mass concentration to carry out ethanol precipitation, standing the solution obtained by the ethanol precipitation in a refrigerator overnight, filtering and concentrating the solution the next day to obtain 200g of crude extract, and finally adding 30g of propylene glycol to obtain the waste tobacco stem extract, wherein the mass ratio of the filtrate to the ethanol is 1:5.
the extracts prepared in examples 1-5 and comparative examples 1-3 were subjected to nicotine content measurement by GC-MS.
The GC/MS analysis conditions were as follows:
gas chromatography conditions: type DB-5 capillary column (30 m × 0.25mm × 0.25 μm); the temperature of a sample inlet is 260 ℃; carrier gas: he; flow rate: 0.96 mL/min; constant voltage mode: 50kPa; temperature rising procedure: keeping the temperature at 50 ℃ for 3min, increasing the temperature to 180 ℃ at 10 ℃/min, keeping the temperature at 20min, increasing the temperature to 260 ℃ at 5 ℃/min, and keeping the temperature for 2min; sample introduction amount: 1 mu L of the solution; the split ratio is as follows: 10:1;
mass spectrum conditions: transmission line temperature: 280 ℃; an ionization mode: EI; ionization energy: 70eV; ion source temperature: 200 ℃; scanning range: 35-600amu; solvent retardation: 3min;
and searching the obtained spectrum by a computer library (NIST 14), selecting a compound with the similarity of more than 90, and comparing the compound with mass spectrograms of all substances to determine the volatile components.
The test results are shown in table 1 below:
TABLE 1 Nicotine content for examples 1-5 and comparative examples 1-3
| Examples | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Nicotine content | 80% | 78% | 79% | 75% | 70% | 65% | 66% | 51% |
As can be seen from the results in Table 1, the yield of the tobacco stem extracts prepared in examples 1 to 5 is significantly higher than that of comparative examples 1 to 3, which shows that the method for extracting tobacco stems provided by the invention can more fully extract the active ingredients in the tobacco stem extracts.
Test example 1
The tobacco stem extracts prepared in the examples 1-5 and the comparative examples 1-3 are used as tobacco leaf additives of cigarettes, the tobacco leaf additives are added into corresponding cigarettes, and cigarette smoking evaluation comparison is carried out, wherein the sensory smoking evaluation method comprises the following steps: blowing out the finished product of the cut tobacco of the cigarette, and balancing under the conditions of temperature (22 +/-1) DEG C and relative humidity (60 +/-2)%. Weighing 8 parts of balanced 30g cut tobacco, marking as A1, A2, A3, A4, A5, D1, D2 and D3, spraying 0.08 mass% of the tobacco stem extracts prepared in the examples 1-5 and the comparative examples 1-3 of the invention in sequence, and then putting the tobacco stem extracts into a constant temperature and humidity box for balancing for 48 hours. The cigarettes were made from the corresponding brands of tobacco tubes and subjected to sensory evaluation with the addition of flavors by a professional panel of 7 persons. The results of the smoking are shown in Table 2.
TABLE 2-evaluation of smoking of the extracts prepared in examples 1 to 5 and comparative examples 1 to 3 after adding to cigarettes
| Reference numerals | Evaluation of aspiration results |
| A1 | Rich and elegant fragrance, soft and smooth smoke, obvious cigar smoke fragrance and long smoke |
| A2 | Rich and elegant fragrance, soft and smooth smoke, obvious cigar fragrance and long smoke |
| A3 | Rich and elegant fragrance, soft and smooth smoke, obvious cigar smoke fragrance and long smoke |
| A4 | Rich and elegant fragrance, soft and smooth smoke, obvious cigar fragrance and long smoke |
| A5 | Rich and elegant fragrance, soft and smooth smoke, obvious cigar smoke fragrance and long smoke |
| B1 | The fragrance is through and the coordination of the fragrance is poor |
| B2 | The fragrance is through and the fragrance coordination is poor |
| B3 | The fragrance is through, contains more obvious wood gas, and has poor fragrance harmony |
As can be seen from the results in Table 2, the extracts prepared in examples 1 to 5, when added to cigarettes, can significantly improve the smoking effect of the cigarettes, the fragrance of the cigarettes is richer and more elegant, the smoke is softer and smoother, the fragrance of cigar cigarettes is more significant, and the smoke is kept long. The extracts prepared in the comparative examples 1 and 2 are added into cigarettes, so that the smoking effect is not obviously improved, and the extracts prepared in the comparative examples 1 and 2 have low content of aroma substances and are insufficient for extracting tobacco stems in the preparation process. And not only the smoking effect is not obviously promoted in the comparative example 3, but also impurity gas is contained, the smoking taste of the cigarette is not pure enough, and the smoking experience is poor.
Therefore, the tobacco stem extract preparation method provided by the invention has the advantages that the extract contains rich active ingredients, has better effects of oxidation resistance, bacteriostasis and the like, has short extraction time and low temperature compared with the traditional extraction method, can fully extract the active ingredients, can well recycle wastes, and has higher economic benefit.
The above-described aspects may be implemented individually or in various combinations, and such variations are within the scope of the present invention.
It should be noted that, in this document, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising a component of 8230means that the element does not exclude the presence of another like element in a process, method, article, or apparatus that comprises the element.
The foregoing is a further detailed description of the invention in connection with specific preferred embodiments and it is not intended to limit the invention to the specific embodiments described. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (10)
1. A method for extracting the waste tobacco stems of cigars is characterized by comprising the following steps:
s1, collecting waste tobacco stems, removing impurities, drying, grinding the tobacco stems into powder by using a plant sample grinder, and sieving the powder by using a 40-mesh sieve for later use;
s2, dissolving the tobacco stalk powder in the S1 in water, adding combined enzyme for enzymolysis (40-50) min, and filtering to obtain an enzymolysis solution;
s3, adding the enzymolysis liquid in the S2 into a sodium hydroxide aqueous solution with the mass concentration of 10-15%, uniformly stirring, standing for 2-3 hours, adding a dilute sulfuric acid solution with the mass concentration of 0.5-3%, heating, refluxing and extracting for 2 hours, filtering the solution, and concentrating under reduced pressure to obtain a concentrated solution;
s4, distilling and extracting the concentrated solution in the S3 to obtain distillate;
and S5, filtering the distillate in the step S4 by using a 0.8-micron filter membrane to obtain a filtrate, adding 70% ethanol by mass concentration to carry out ethanol precipitation, standing the solution obtained by ethanol precipitation in a refrigerator overnight, filtering and concentrating the next day to obtain a crude extract, and finally adding propylene glycol to obtain the waste tobacco stem extract.
2. The method for extracting the waste tobacco stems of the cigars as claimed in claim 1, wherein the tobacco stems in the S1 are dried in a forced air drying oven at 40-42 ℃ for 11-12 h.
3. The method for extracting the waste tobacco stems of the cigars according to claim 1, wherein the mass ratio of the combined enzymes in the S2, including pectinase, cellulase and protease, is 1:1:1.
4. the method for extracting the waste tobacco stems of the cigars according to claim 1, wherein the mass ratio of the tobacco stem powder, the water and the combined enzyme in the S2 is 40:400: (0.4-2).
5. The method for extracting the waste tobacco stems of the cigars according to claim 1, wherein the mass ratio of the enzymolysis liquid, the sodium hydroxide aqueous solution and the dilute sulfuric acid solution in the S3 is (4-5): 1: (15-20).
6. The method for extracting the waste tobacco stems of the cigars according to claim 1, wherein the extracting solution distilled and extracted in the step S4 is an ethanol solution with a mass concentration of 70%.
7. The method for extracting the waste tobacco stems of the cigars according to claim 1, wherein the mass ratio of the concentrated solution to the extracting solution in the step S4 is 1:10.
8. the method for extracting the waste tobacco stems of the cigars as claimed in claim 1, wherein the distillation extraction temperature in the step S4 is (70-72) DEG C, and the extraction time is 1h.
9. The method for extracting the waste tobacco stems of the cigars according to claim 1, wherein the mass ratio of the filtrate to the ethanol in the step S5 is 1:5.
10. the method for extracting the waste tobacco stems of the cigars according to claim 1, wherein the mass ratio of the crude extract in the S5 to the propylene glycol is 100:15.
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