CN115399498A - Tobacco extract, preparation method thereof and tobacco product - Google Patents
Tobacco extract, preparation method thereof and tobacco product Download PDFInfo
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- CN115399498A CN115399498A CN202211039131.1A CN202211039131A CN115399498A CN 115399498 A CN115399498 A CN 115399498A CN 202211039131 A CN202211039131 A CN 202211039131A CN 115399498 A CN115399498 A CN 115399498A
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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
- A24B15/241—Extraction of specific substances
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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
- A24B15/241—Extraction of specific substances
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Abstract
The invention relates to a tobacco extract, a preparation method thereof and a tobacco product. The preparation method of the tobacco extract comprises the following steps: drying and crushing tobacco raw materials to obtain tobacco powder; carrying out ultrasonic washing on the tobacco powder for 1-3 times by using deionized water, and sequentially carrying out filtration and centrifugal dehydration after each ultrasonic washing to obtain washing residues; drying the water washing residues to obtain low-nicotine tobacco powder; performing primary carbon dioxide supercritical extraction on the low nicotine tobacco powder to obtain a primary extract; continuously performing secondary carbon dioxide supercritical extraction on the residue subjected to the primary carbon dioxide supercritical extraction to obtain a secondary extract; and combining the first extract and the second extract to obtain the tobacco extract. The preparation method of the tobacco extract enables the endogenous fragrant components of tobacco and nicotine to be separated, the fragrant components of tobacco are not damaged, the nicotine content in the extract is extremely low, the content of the fragrant components is greatly improved, the preparation cost is low, the quality of the spice is good, and no solvent residue exists.
Description
Technical Field
The invention relates to the technical field of tobacco extracts, in particular to a tobacco extract, a preparation method thereof and a tobacco product.
Background
The tobacco extract is derived from tobacco, and according to the homologous quality, the tobacco natural aroma with different styles can be obtained by selecting tobacco leaf raw materials with different types and flavor styles. The tobacco extract is the most important component of the tobacco flavor and fragrance, and mainly comprises the following components: tobacco essential oil, tobacco absolute oil, tobacco extract, tobacco tincture, supercritical (sub) critical fluid tobacco extract, tobacco non-enzymatic browning product, tobacco thermal processing product, tobacco unconcentrated extract and the like. The mandatory national standard of GB 41700-2022E-cigarette definitely stipulates that the characteristic flavor of the product should not be presented with other flavors except tobacco, and definitely requires: the aerosol should contain nicotine, the electronic cigarette product without nicotine should not be sold on the market, but nicotine extracted from tobacco must be used, and the concentration of nicotine in the aerosol should not be higher than 20mg/g, and the total amount should not be higher than 200mg.
Nicotine is a main alkaloid in tobacco, accounts for more than 90 percent of total alkaloid in the tobacco, and has the Nicotine content of about 1.5 to 3.5 percent and is as high as 3.5 to 5.5 percent in burley tobacco, and the appropriate Nicotine content in the cigarette can improve the strength, the alcohol taste and the taste, relieve the stimulation and improve the spirit and eliminate the fatigue by proper intake, but excessive intake can induce addiction and damage the health of human bodies.
Disclosure of Invention
In order to solve or partially solve the problems in the related art, the invention provides a tobacco extract, a preparation method thereof and a tobacco product.
The invention provides a preparation method of a tobacco extract, which comprises the following steps:
step a), drying and crushing tobacco raw materials to obtain tobacco powder;
b), carrying out ultrasonic washing on the tobacco powder for 1-3 times by using deionized water, and sequentially filtering and centrifugally dewatering after each ultrasonic washing to obtain washing residues;
step c), drying the washing residues to obtain low-nicotine tobacco powder;
step d), carrying out primary carbon dioxide supercritical extraction on the low nicotine tobacco powder to obtain a primary extract;
step e), continuously carrying out secondary carbon dioxide supercritical extraction on the residue subjected to the primary carbon dioxide supercritical extraction to obtain a secondary extract; the temperature of the secondary supercritical extraction is 80-100 ℃, and the pressure is 20-30 MPa;
and f) combining the primary extract and the secondary extract to obtain the tobacco extract.
Further, the step a) is specifically that the tobacco raw material is dried for 1-2 hours at the temperature of 40-60 ℃, and is crushed to 20-40 meshes to obtain the tobacco powder.
Further, in the step b), in each ultrasonic water washing, the mass ratio of the deionized water to the tobacco powder is (10-50): 1, the ultrasonic time is 20-40 min, and the ultrasonic frequency is 30 KHz-60 KHz.
Further, in the step c), the water content of the low nicotine tobacco powder is 10% -15%.
Further, the conditions of the primary supercritical carbon dioxide extraction in the step d) are as follows:
the extraction temperature is 40-60 ℃, the extraction pressure is 10-30 MPa, and the extraction time is 1-3 h.
Further, in the step d), absolute ethyl alcohol is used as an entrainer in the extraction process; the weight volume ratio of the low nicotine tobacco powder to the absolute ethyl alcohol is 1g (0.1 mL-0.25 mL).
Further, the conditions of the secondary carbon dioxide supercritical extraction in the step e) are as follows:
the extraction temperature is 80-100 ℃, the extraction pressure is 20-30 MPa, the circular extraction is carried out, and the extraction time is 1-2 h.
Further, in the step e), absolute ethyl alcohol is used as an entrainer in the extraction process; the weight volume ratio of the low nicotine tobacco powder to the absolute ethyl alcohol is 1g (0.05 mL-0.125 mL).
The invention also provides a tobacco extract, which is prepared according to any one of the methods.
Correspondingly, the invention also provides a tobacco product which contains the tobacco extract.
The preparation method of the tobacco extract provided by the invention can have the following beneficial effects:
1. the method provided by the invention uses deionized water to carry out ultrasonic water washing treatment on the tobacco raw material for 1-3 times in advance, so that nicotine and part of macromolecular impurities in tobacco powder can be dissolved, and nonpolar fragrance components are not lost; experiments prove that the nicotine content of the tobacco extract prepared by the method provided by the invention is extremely low, the nicotine content in the extract after primary ultrasonic water washing is lower than 0.5%, the nicotine content after secondary ultrasonic water washing is lower than 0.1%, and the nicotine content after tertiary ultrasonic water washing is lower than 0.05%.
2. The method provided by the invention carries out ultrasonic washing treatment on the tobacco raw material in advance, can also loosen the tissue structure of the treated tobacco powder, and is more favorable for improving the supercritical CO 2 And (4) extracting yield of the endogenous fragrant components by the fluid.
3. After the method provided by the invention is used for carrying out primary carbon dioxide supercritical extraction, secondary supercritical extraction is carried out on residues at a higher temperature, the temperature is increased to accelerate the degradation speed of the fragrance precursor and generate a plurality of micromolecular aldehyde ketone and ester fragrance substances, the temperature is continuously increased, the Maillard reaction is accelerated, and the content of Maillard reactants such as furanone, pyrone and pyrrole substances is rapidly increased, so that the loss of water-soluble aldehyde ketone compounds caused by ultrasonic water washing can be compensated, more fragrance component substances are generated, the fragrance is enriched, the prepared spice presents more prominent 'sweet taste' in taste, the back sweet feeling of cigarette smoke is promoted, and the taste characteristics of 'sweet' and 'moist' of cigarettes are highlighted;
in conclusion, the preparation method of the tobacco extract provided by the invention enables the endogenous aroma components of the tobacco and nicotine to be separated, the aroma components of the tobacco are not damaged, the nicotine content in the extract is extremely low, the content of the aroma components is greatly improved, the preparation cost is low, the quality of the spice is good, and no solvent residue exists.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as claimed.
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The above and other objects, features and advantages of the present invention will become more apparent by describing in detail exemplary embodiments thereof with reference to the attached drawings, wherein like reference numerals generally represent like parts in the exemplary embodiments of the present invention.
FIG. 1 is a GC/MS plot of extract 0, extract 1 and extract 2 of example 1 of the present invention;
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this specification and the appended claims, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any and all possible combinations of one or more of the associated listed items.
It should be understood that although the terms "first", "second", "third", etc. may be used herein to describe various information, these information should not be limited to these terms. These terms are only used to distinguish one type of information from another. For example, first information may also be referred to as second information, and similarly, second information may also be referred to as first information, without departing from the scope of the present invention. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The invention provides a preparation method of a tobacco extract, which comprises the following steps:
step a), drying and crushing tobacco raw materials to obtain tobacco powder;
b), carrying out ultrasonic washing on the tobacco powder for 1-3 times by using deionized water, and sequentially filtering and centrifugally dewatering after each ultrasonic washing to obtain washing residues;
step c), drying the washing residues to obtain low-nicotine tobacco powder;
step d), carrying out primary carbon dioxide supercritical extraction on the low nicotine tobacco powder to obtain a primary extract;
step e), continuously carrying out secondary carbon dioxide supercritical extraction on the residue subjected to the primary carbon dioxide supercritical extraction to obtain a secondary extract; the temperature of the secondary supercritical extraction is 80-100 ℃, and the pressure is 20-30 MPa;
and f) combining the primary extract and the secondary extract to obtain the tobacco extract.
The step a) is a step of pretreating the tobacco raw material to be processed into powder for the subsequent processes of water washing and supercritical extraction. The step can be specifically as follows: the tobacco raw material is dried for 1-2 h at 40-60 ℃ and crushed to 20-40 meshes to obtain the tobacco powder. The tobacco raw materials can be tobacco and tobacco products such as tobacco leaves, tobacco powder, tobacco stems and the like generated in the processes of tobacco leaf cultivation, transportation, threshing and redrying and rolling.
And step b) is a step of carrying out ultrasonic washing on the tobacco powder obtained after pretreatment. The nicotine belongs to a water-soluble component, and the main purpose of the ultrasonic water washing in the step is to remove the nicotine in the tobacco powder, so that the content of the nicotine in the tobacco extract obtained by subsequent extraction is reduced. In addition, the cavity effect generated by the ultrasonic can also make the tissue of the tobacco powder more loose, which is beneficial to improving the subsequent supercritical CO 2 And (4) the extraction yield of the fluid to the endogenous fragrant components.
In this step, the reason why the ultrasonic medium is deionized water is as follows: on one hand, the deionized water is a polar solvent, nicotine and part of macromolecular impurities in the tobacco powder can be dissolved, nonpolar fragrance components are not lost, on the other hand, the tobacco powder treated by the deionized water still contains certain moisture after being dried, and histiocyte collapse becomes loose after the tobacco powder removes part of macromolecules such as sugar, protein and starch, and the yield of the fragrance components extracted by the carbon dioxide supercritical extraction is higher. The ultrasonic water washing is carried out for 1-3 times in total, the nicotine content in the washing residue is in a descending trend along with the increase of the ultrasonic water washing times, but when the water washing times exceed 3 times, the nicotine content in the washing residue is extremely low and is generally lower than 0.05 percent; in addition, when the nicotine is removed by ultrasonic water washing, flavor substances such as water-soluble aldehyde ketone compounds can be lost; and the inventors of the present application found that the content of a part of aroma-forming compounds in the extract becomes lower as the number of times of washing with water increases. In summary, the total times of ultrasonic washing is set to be 1-3 times. As a preferable scheme of this embodiment, in each ultrasonic water washing, the mass ratio of the deionized water to the tobacco powder is (10-50): 1, the ultrasonic time is 20min to 40min, and the ultrasonic frequency is 30KHz to 60KHz; more preferably, the mass ratio of the deionized water to the tobacco powder is (25-40): 1, the ultrasonic time is 30min, and the ultrasonic frequency is 40KHz. The number of times of the particular ultrasonic water wash can be selected by one skilled in the art according to particular needs.
Step c) is a process of further drying the washing residue after ultrasonic washing and dehydration treatment, and the drying has the following effects: the tobacco powder after washing still contains higher water, when the water content is too high, a water film is easily formed on the surface of the material, the mass transfer of the supercritical carbon dioxide and the material is influenced, the material is easy to agglomerate, the extraction time is prolonged, and the extraction yield is reduced. The inventor of the application discovers that the moisture content of the tobacco powder subjected to ultrasonic water washing has an influence on supercritical extraction, when the moisture content of the material is higher than 15%, the extraction yield is obviously reduced, and the extract has a water layer, so that the amount of part of flavor components is reduced. Furthermore, the water content of the low-nicotine tobacco powder obtained after drying is controlled to be 10% -15%, and the supercritical extraction effect of the low-nicotine tobacco powder with the water content is optimal, so that the water content of the low-nicotine tobacco powder in the step is preferably 10% -15%. The preferred procedure is as follows: and drying the washing residues at 40-60 ℃ until the water content is 10% -15%, thus obtaining the low nicotine tobacco powder.
Step d) is to carry out the first carbon dioxide supercritical extraction on the low nicotine tobacco powder obtained by drying, wherein the carbon dioxide supercritical extraction does not use or uses a small amount of organic solvent, and the extractant carbon dioxide can be recycled, so that the method is safe and environment-friendly; moreover, the extraction can be carried out at low temperature, and heat-sensitive aroma components can also be extracted. In this embodiment, the substances such as alcohols, acids, esters, aldehydes and ketones, alkanes and the like in the low nicotine tobacco powder can be extracted by performing the supercritical extraction once. And (3) after the first supercritical extraction, desolventizing the materials in the separation kettle to obtain a first extract. Preferably, the conditions of the supercritical carbon dioxide extraction in the first step are as follows: the extraction temperature is 40-60 ℃, the extraction pressure is 10-30 MPa, the circular extraction is carried out, and the extraction time is 1-3 h. More preferably, the extraction temperature is 45 ℃, the extraction pressure is 30MPa, the circulating extraction is carried out, and the extraction time is 1.5 h-2 h. As a preferred scheme of the embodiment, in the extraction process, absolute ethyl alcohol is preferably used as an entrainer, and the ethyl alcohol is an excellent solvent, has good dissolving capacity for strong and weak aroma components, has a boiling point of 78.3 ℃, is non-toxic, and is a permissible solvent for cigarette flavoring. Furthermore, the weight volume ratio of the low nicotine tobacco powder to the absolute ethyl alcohol is 1g (0.1 mL-0.25 mL). The absolute ethyl alcohol can be added into the extract in advance before the carbon dioxide fluid is introduced to be mixed with the low nicotine tobacco powder, and can also be introduced into the extraction kettle along with the carbon dioxide fluid.
The step e) is a step of continuously performing secondary carbon dioxide supercritical extraction on the residue after the primary extraction. Although the supercritical water washing in the step a) is beneficial to removing nicotine, part of water-soluble aldehyde ketone compounds in the tobacco powder are lost along with the supercritical water washing, and in order to compensate the loss of the compounds, the secondary supercritical extraction is carried out in the step, and compared with the primary supercritical extraction, the extraction temperature is higher, the temperature is 80-100 ℃, and the pressure is 20-30 MPa. The flavor substances and the precursor thereof in the tobacco are complex and various in variety, the degradation speed of the flavor precursor can be accelerated by raising the temperature, some micromolecule aldehyde ketone and ester flavor substances are generated, the temperature is continuously raised, the Maillard reaction is accelerated, and the content of Maillard reactants such as furanone, pyrone and pyrrole substances is rapidly increased, so that the loss of water-soluble aldehyde ketone compounds caused by ultrasonic water washing can be compensated, more flavor component substances are generated, and the aroma is enriched. In this step, the conditions of the secondary carbon dioxide supercritical extraction are as follows: the extraction temperature is 80-100 ℃, the extraction pressure is 20-30 MPa, the circular extraction is carried out, and the extraction time is 1-2 h. In this step, the extraction temperature has an influence on the composition of the flavor components, and if the temperature is too low, the flavor components are less in content, and if the temperature is too high, scorched bitter components are generated, and the extraction temperature is more preferably 95 to 100 ℃, and most preferably 95 ℃; the extraction pressure is most preferably 30MPa. Similar to the first supercritical extraction, anhydrous ethanol is also preferably used as an entrainer in this step. Furthermore, the weight volume ratio of the low nicotine tobacco powder to the absolute ethyl alcohol is 1g (0.05 mL-0.125 mL).
And (e) after the secondary supercritical extraction, desolventizing the feed liquid in the separation kettle to obtain a secondary extract, and then combining the primary extract and the secondary extract according to the step f) to obtain the tobacco extract, wherein the tobacco extract is low in nicotine content and high in endogenous aroma component content.
From the above, the preparation method of the tobacco extract provided by the invention has the following advantages:
1. the method provided by the invention uses deionized water to carry out ultrasonic water washing treatment on the tobacco raw material for 1-3 times in advance, so that nicotine and part of macromolecular impurities in tobacco powder can be dissolved, and nonpolar fragrance components are not lost; experiments prove that the nicotine content of the tobacco extract prepared by the method provided by the invention is extremely low, the nicotine content in the extract after primary ultrasonic water washing is lower than 0.5%, the nicotine content after secondary ultrasonic water washing is lower than 0.1%, and the nicotine content after tertiary ultrasonic water washing is lower than 0.05%.
2. The method provided by the invention carries out ultrasonic washing treatment on the tobacco raw material in advance, can also loosen the tissue structure of the treated tobacco powder, and is more favorable for improving the supercritical CO 2 And (4) the extraction yield of the fluid to the endogenous fragrant components.
3. After the method provided by the invention is used for carrying out primary carbon dioxide supercritical extraction, secondary supercritical extraction is carried out on residues at a higher temperature, the temperature is increased to accelerate the degradation speed of the fragrance precursor and generate a plurality of micromolecular aldehyde ketone and ester fragrance substances, the temperature is continuously increased, the Maillard reaction is accelerated, and the content of Maillard reactants such as furanone, pyrone and pyrrole substances is rapidly increased, so that the loss of water-soluble aldehyde ketone compounds caused by ultrasonic water washing can be compensated, more fragrance component substances are generated, the fragrance is enriched, the prepared spice presents more prominent 'sweet taste' in taste, the back sweet feeling of cigarette smoke is promoted, and the taste characteristics of 'sweet' and 'moist' of cigarettes are highlighted;
in conclusion, the preparation method of the tobacco extract provided by the invention enables the endogenous aroma components of the tobacco and nicotine to be separated, the aroma components of the tobacco are not damaged, the nicotine content in the extract is extremely low, the content of the aroma components is greatly improved, the preparation cost is low, the quality of the spice is good, and no solvent residue exists.
The technical scheme of the invention is further explained by combining specific examples as follows:
example 1 Effect of the number of ultrasonic Water washes on Low temperature supercritical extraction
1. Collecting tobacco powder generated in the rolling process, drying the tobacco powder at 40 ℃ for 1h, crushing and sieving by a 20-mesh sieve for later use;
2. weighing 1kg of tobacco powder, putting into a flask, adding 25 mass times of deionized water, carrying out ultrasonic treatment at the frequency of 40KHz for 30min at normal temperature, filtering, collecting a first filtrate, and carrying out centrifugal dehydration on the tobacco powder to obtain a first residue; weighing 600g of first residues, adding 25 mass times of deionized water, carrying out ultrasonic treatment for 30min, filtering, collecting second filtrate, and carrying out centrifugal dehydration on tobacco powder to obtain second residues; adding 25 mass times of deionized water into 300g of the second residue, carrying out ultrasonic treatment for 30min, filtering, collecting a third filtrate, and carrying out centrifugal dehydration on the tobacco powder to obtain a third residue.
3. Respectively further drying the first residue, the second residue and the third residue at 60 ℃ to obtain first low nicotine tobacco powder, second low nicotine tobacco powder and third low nicotine tobacco powder with the water content of about 12%;
4. weighing 200g of dried first low-nicotine tobacco powder, placing into an extraction kettle, adding 50mL of anhydrous ethanol, setting the extraction pressure at 30MPa and the temperature at 45 ℃, and introducing CO 2 (ii) a Pressurizing to set pressure, circularly extracting for 1.5h, and collecting to obtain tobacco supercritical CO 2 And (3) extracting. Since this embodiment only analyzes the influence of the ultrasonic washing times on the low-temperature carbon dioxide supercritical extraction effect, this embodiment does not perform the step of secondary carbon dioxide supercritical extraction.
Sequentially carrying out CO treatment on the raw tobacco powder, the first low-nicotine tobacco powder, the second low-nicotine tobacco powder and the third low-nicotine tobacco powder which are not subjected to ultrasonic washing according to the method 2 Supercritical fluid extraction to respectively obtain corresponding supercritical CO 2 A tobacco extract. Mixing the raw tobacco powder, the first low nicotine tobacco powder, the second low nicotine tobacco powder and the third low nicotine tobaccoThe supercritical CO of the powder 2 The tobacco extracts are labeled as extract 0, extract 1, extract 2 and extract 3 in sequence.
Taking equal amount of above tobacco extract, adding 100 μ L of 10mg/mL ethyl salicylate as internal standard, diluting to 5mL, collecting appropriate amount of solution, filtering, and performing GC/MS analysis, wherein the result is shown in FIG. 1 (since FIG. 1 mainly shows the variation of nicotine content in each extract, and the nicotine content of the extract after two times of ultrasonic water washing is very low, the GC/MS graph of the extract after three times of ultrasonic water washing is not shown in FIG. 1)
The relative content of each aroma component in extract 0 was taken as reference 1, and the change rates of each aroma component in comparative extract 0, extract 1, extract 2 and extract 3 were analyzed, and the results are shown in table 1.
TABLE 1 comparison of the aroma components in tobacco extracts (times)
As can be seen from Table 1:
1) The loss of part of water-soluble flavor components (because the raw materials are crushed in the cigarette production process, and the flavor components such as propylene glycol, glycerol, some aldehyde ketone and the like are introduced during flavoring and feeding) after one-time washing can not be basically detected;
2) Small parts of components such as micromolecular benzoic acid, phenylacetic acid, solanone, scopoletin and the like are basically not influenced by water washing treatment;
3) The content of most endogenous fragrant components in the tobacco is improved to different degrees after ultrasonic water washing for one time, two times and three times;
4) The content of part of endogenous aroma components in the tobacco is obviously improved after one-time washing; for example: the contents of beta-damascenone, geranylacetone, 4,7, 9-megastigmatrienol-3-one, neophytadiene, palmitic acid, methyl palmitate, benzyl benzoate, methyl linolenate, plant alcohol, pentadecanoic acid, stearic acid, higher alkane, squalene, vitamin E and the like are increased by more than 2 times, especially megastigmatrienone, namely tobacco leaf ketone, shows lasting sweet tobacco fragrance and is an important component of natural fragrance of flue-cured tobacco, the cigarette flavoring agent can play a role by being added in a small amount, and the content of the cigarette is increased by more than 3 times after being washed by water for once; the beta-damascenone is also an extremely important aroma component in tobacco, can sweeten and mellow smoke, improve bad smell, increase natural feeling and thick feeling, and increase the content by about 3 times after once water washing treatment; the total amount of long-chain fatty acid esters such as methyl palmitate, ethyl palmitate, methyl linolenate, methyl myristate and methyl stearate is increased by several times, and the fatty acid esters can endow cigarettes with faint scent and soft smoke and increase the faint scent of the cigarettes; the high-grade alkane is the main component of the tobacco leaf wax, can inhibit the loss of moisture, plays a role in moisture retention, and the content of the high-grade alkane is also obviously increased after washing; the content of squalene with harm reduction effect is increased by about 5 times after one-time water washing; the vitamin E can reduce the damage of harmful components in the smoke on DNA, and the extraction amount is greatly increased after washing;
5) The nicotine content is respectively reduced by about 90 percent, 97 percent and 99 percent after the first ultrasonic water washing, the second ultrasonic water washing and the third ultrasonic water washing.
This example is used to illustrate the effect of water washing and the number of water washing on the flavor components of tobacco powder extracted by supercritical carbon dioxide, the extract has been separated, the second supercritical extraction step is performed on the basis of this step, the tobacco powder after the first supercritical extraction is extracted continuously after being heated, and the obtained extracts are combined to obtain the tobacco extract of the present invention.
Example 2 Effect of temperature of high temperature supercritical extraction on extraction efficiency
1. Putting the tobacco leaf raw material into a 60 ℃ oven for drying for 2h to obtain the water content of about 10%, and then crushing the tobacco leaf raw material into 20-mesh tobacco powder for later use;
2. weighing 200g of dry tobacco powder residues, placing into an extraction kettle, adding 50mL of anhydrous ethanol, setting the extraction pressure at 30MPa and the temperature at 45 ℃, and introducing CO 2 Pressurizing to set pressure, circularly extracting for 2 hr, decompression desolventizing the residue in the extraction kettle, and introducing CO 2 And 20mL of absolute ethyl alcohol, continuously performing secondary supercritical extraction for 1h at 100 ℃ under the condition of 30MPa, and collecting to obtain supercritical CO 2 Tobacco extract, labeled extract G.
3. Repeating the above steps, with the difference that the temperature of the secondary supercritical extraction is 35 deg.C, 45 deg.C, 55 deg.C, 65 deg.C, 75 deg.C, and 85 deg.C respectively, and collecting the supercritical CO 2 The tobacco extracts are labeled as extract A, extract B, extract C, extract D, extract E, and extract F, respectively.
Respectively taking equal amount of the extracts, adding 100 mu L of 10mg/mL ethyl salicylate as an internal standard, fixing the volume to 5mL by absolute ethyl alcohol, filtering by a micro-membrane, and performing GC/MS analysis, wherein the content of various aroma substances in the extracts is listed in Table 2.
The relative content of each aroma component in the extract a is taken as reference 1, the content change rate of each aroma substance in the comparative extracts B to G is analyzed, and the results are listed in table 3.
TABLE 2 content of various aroma substances (mg) in the extract
TABLE 3 comparison of the content of aroma components in the extracts (times)
As can be seen from tables 2 and 3: the total extraction amount of furan and pyranone cyclic aldehyde ketone compounds in the extract is obviously increased at 85 ℃ and is increased by 260 percent to 100 ℃, wherein 3, 5-dihydroxy-2-methyl-4H-pyran-4-ketone is increased by 230 percent, and the extraction amount of 2, 3-dihydro-3, 5-dihydroxy-6-methyl-4 (H) -pyran-4-ketone (DDMP) is increased by about 7 times from 80 to 100 ℃. The ketone substances have good water solubility, present prominent sweet taste in taste sense, can improve the sweet feeling of cigarette smoke, and show the taste characteristics of 'sweet' and 'moist'. The extraction amount of main aroma substances in tobacco, such as solanone, geranyl acetone, farnesyl acetone, megastigmatrienone, 4-hydroxy-beta-dihydrodamascenone, 1-hydroxy-4-ketone-2-ionone and the like, at the temperature of 80-100 ℃ is also improved by 30-100%.
It should be noted that, this embodiment is used to verify the influence of the secondary supercritical extraction temperature on the extraction effect, and in order to simplify the experimental process, the step of ultrasonic water washing is omitted, but the influence of the secondary supercritical extraction temperature on the extraction effect is not influenced and described.
Example 3 Effect of Material moisture content before extraction on supercritical extraction
1. Collecting tobacco powder generated in the rolling process, adding deionized water in an amount which is 35 times the weight of the tobacco powder, carrying out ultrasonic treatment at the frequency of 40KHz for 30min at normal temperature, filtering, collecting first filtrate, and carrying out centrifugal dehydration on the tobacco powder to obtain tobacco powder residues;
2. placing the washed tobacco powder residues in a 60 ℃ oven to be respectively dried until the moisture content is about 5 percent, 10 percent, 15 percent and 20 percent for later use;
3. weighing 200g of tobacco powder residue with water content of about 5%, placing in an extraction kettle, setting extraction pressure at 30MPa and temperature at 45 deg.C, and introducing CO 2 Pressurizing to set pressure, circularly extracting for 2h, and collecting to obtain supercritical CO 2 Extracting tobacco extract as extract I sequentially by the same methodThe tobacco powder residue containing water of about 10%,15%, 20% is respectively labeled as extract II, extract III, and extract IV.
The extracts were subjected to GC/MS analysis after treatment as described in example 2, and the relative amounts of the various aroma substances in the extracts are given in Table 4.
TABLE 4 quality of aroma (mg) in the extracts of the various classes
| Extract I | Extract II | Extract III | Extract IV | |
| Water content ratio | 5％ | 10％ | 15％ | 20％ |
| Alcohols | 3.53 | 3.46 | 4.15 | 3.55 |
| Organic acids | 0.84 | 1.32 | 1.94 | 0.43 |
| Esters of unsaturated carboxylic acids | 0.65 | 0.66 | 0.85 | 0.84 |
| Aldehyde ketones | 0.27 | 0.38 | 0.59 | 0.57 |
| Heterocyclic rings | 1.03 | 3.32 | 3.66 | 5.47 |
| Alkanes and their use as pesticides | 4.44 | 2.72 | 2.78 | 2.71 |
| Terpenes as pesticides | 3.46 | 4.10 | 4.00 | 3.02 |
| Total amount of | 14.22 | 15.96 | 17.97 | 16.59 |
| Extraction yield/% | 1.45 | 2.05 | 2.17 | 1.86 |
| Amount of fragrance compound | 87 | 108 | 108 | 105 |
From table 4 it can be seen that: after the tobacco powder is dried, the total extraction amount of the fragrant substances is lower, and the contents of alcohols, small molecular acids, aldehyde ketone and the like with low boiling points are obviously reduced. With the increase of the water content, the extraction yield of the perfume and the number of the fragrant compounds are increased, and the most increased extraction amount is esters, especially dihydroactinidiolide, DL-panthenolide, scopoletin and the like; 2, 3-dihydro-3, 5 dihydroxy-6-methyl-4 (H) -pyran-4-one (DMPP), methylcyclopentenone (MCP), 5-hydroxymethylfurfural and the like having a burnt and sweet aroma increase with increasing moisture content of the tobacco ends; terpenoids such as neophytadiene and squalene gradually decrease with increasing water content. Therefore, the material contains a proper amount of water to improve the performance of the supercritical fluid and be beneficial to improving the solubility of the polar hydrophilic fragrant substances, but when the water content is too high, the material in the extraction kettle is wet and is easy to agglomerate under high pressure, so that the extraction yield of part of fragrant ingredients is reduced.
It should be noted that, this embodiment is used to verify the influence of the water content of the material before extraction on the supercritical extraction effect, and therefore, although the steps of ultrasonic water washing and high-temperature supercritical extraction are omitted, the influence of the water content of the material before extraction on the supercritical extraction is not affected.
Example 4
1. Collecting tobacco powder generated in the rolling process, drying the tobacco powder at 40 ℃ for 1h, crushing and sieving with a 20-mesh sieve for later use;
2. weighing 1kg of tobacco powder, putting into a flask, adding deionized water in an amount which is 40 times the weight of the tobacco powder, carrying out ultrasonic treatment at the frequency of 40KHz for 30min at normal temperature, filtering, collecting filtrate, and carrying out centrifugal dehydration on the tobacco powder to obtain tobacco powder residues; further drying the tobacco powder residue at 60 ℃ to obtain tobacco powder with the water content of about 15% for later use;
3. weighing 200g of the tobacco powder treated above, placing the tobacco powder into an extraction kettle, adding 50mL of absolute ethyl alcohol, setting the extraction pressure at 30MPa and the temperature at 45 ℃, and introducing CO 2 Pressurizing to a set pressure, circularly extracting for 1.5h, decompressing and desolventizing residues in the extraction kettle, heating to 95 ℃, and introducing 20mL of absolute ethyl alcohol and CO 2 Continuously performing secondary supercritical extraction for 1.5h under the condition of 30MPa, mixing and collecting to obtain tobacco powder supercritical CO 2 And (3) extracting.
4. Performing CO treatment on raw tobacco powder which is not subjected to ultrasonic water washing according to the method 2 Supercritical extraction to obtain corresponding supercritical CO 2 A tobacco extract. Subjecting the above supercritical CO of the original tobacco powder and the tobacco powder after primary washing 2 The tobacco extracts are labeled as extract X, extract Y in sequence.
Taking 0.1g of the extract X and the extract Y, respectively adding 100 mu L of 10mg/mL ethyl salicylate as an internal standard, adding absolute ethyl alcohol to a constant volume of 5mL, taking a proper amount of solution, filtering the solution through a 0.45 mu m organic phase filter membrane, and performing GC/MS analysis. The relative amounts of each aroma component in extract X and extract Y are shown in table 5.
TABLE 5 content (mg) of some aroma components in the extract
Table 5 shows that: the tobacco powder is subjected to primary supercritical extraction at low temperature after being washed once, the temperature of the extracted material is raised, and secondary supercritical extraction is continuously performed.
Observing the appearance, wherein the extract X has uniform color and is orange yellow; through the evaluation of the fragrance of the spices, the tobacco fragrance, fresh and sweet fragrance and baking fragrance of the extract X are outstanding, and the tobacco fragrance is purer and more natural.
The organic combination of different flavor components forms the flavor characteristics of the flavor, so that the tobacco source flavor with strong applicability can be prepared by adjusting the washing times and the extraction conditions in a certain range according to the content of nicotine in the tobacco powder and combining the flavoring test result, and the cigarette flavor blending and the self-guarantee capability of the flavor and the flavor are promoted.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is chosen in order to best explain the principles of the embodiments, the practical application, or improvements made to the technology in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
Claims (10)
1. A method for preparing a tobacco extract, comprising:
step a), drying and crushing tobacco raw materials to obtain tobacco powder;
b), carrying out ultrasonic water washing on the tobacco powder for 1-3 times by using deionized water, and sequentially filtering and centrifugally dewatering after each ultrasonic water washing to obtain washing residues;
step c), drying the washing residues to obtain low-nicotine tobacco powder;
step d), carrying out primary carbon dioxide supercritical extraction on the low nicotine tobacco powder to obtain a primary extract;
step e), continuously performing secondary carbon dioxide supercritical extraction on the residue subjected to the primary carbon dioxide supercritical extraction to obtain a secondary extract; the temperature of the secondary supercritical extraction is 80-100 ℃, and the pressure is 20-30 MPa;
and f), combining the primary extract and the secondary extract to obtain the tobacco extract.
2. The preparation method according to claim 1, wherein the step a) is specifically that the tobacco raw material is dried at 40-60 ℃ for 1-2 h and crushed to 20-40 meshes to obtain the tobacco powder.
3. The preparation method according to claim 1, wherein in the step b), the mass ratio of the deionized water to the tobacco powder in each ultrasonic water washing is (10-50): 1, the ultrasonic time is 20-40 min, and the ultrasonic frequency is 30 KHz-60 KHz.
4. A method as claimed in claim 1, wherein in step c), the low nicotine tobacco powder has a moisture content of 10-15%.
5. The preparation method according to claim 1, wherein the conditions of the primary supercritical carbon dioxide extraction in step d) are as follows:
the extraction temperature is 40-60 ℃, the extraction pressure is 10-30 MPa, and the extraction time is 1-3 h.
6. The preparation method according to claim 5, wherein in the step d), absolute ethyl alcohol is used as an entrainer in the extraction process; the weight volume ratio of the low nicotine tobacco powder to the absolute ethyl alcohol is 1g (0.1 mL-0.25 mL).
7. The preparation method according to claim 1, wherein the conditions of the secondary supercritical carbon dioxide extraction in step e) are as follows:
the extraction temperature is 80-100 ℃, the extraction pressure is 20-30 MPa, and the extraction time is 1-2 h.
8. The preparation method of claim 7, wherein in the step e), absolute ethyl alcohol is used as an entrainer in the extraction process; the weight volume ratio of the low nicotine tobacco powder to the absolute ethyl alcohol is 1g (0.05 mL-0.125 mL).
9. A tobacco extract, characterized in that it is prepared according to the method of any one of claims 1 to 8.
10. A tobacco product comprising the tobacco extract of claim 9.
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| CN103183585A (en) * | 2012-12-10 | 2013-07-03 | 青岛研博电子有限公司 | Method for extracting solanesol by combining ultrasonic enzymic method and supercritical carbon dioxide |
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