CN115399498B - Tobacco extract, preparation method thereof and tobacco product - Google Patents
Tobacco extract, preparation method thereof and tobacco product Download PDFInfo
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- CN115399498B CN115399498B CN202211039131.1A CN202211039131A CN115399498B CN 115399498 B CN115399498 B CN 115399498B CN 202211039131 A CN202211039131 A CN 202211039131A CN 115399498 B CN115399498 B CN 115399498B
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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 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 carbon dioxide supercritical extraction on the low-nicotine tobacco powder for the first time to obtain a first extract; carrying out secondary carbon dioxide supercritical extraction on the residue after the primary carbon dioxide supercritical extraction to obtain a secondary extract; combining the primary extract and the secondary extract to obtain the tobacco extract. The preparation method of the tobacco extract enables endogenous aroma components of tobacco and nicotine to be separated, the aroma components of the tobacco are not destroyed, the content of the nicotine 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.
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 homologous homogeneity, tobacco natural fragrance of different styles can be obtained through selecting tobacco raw materials of different types and fragrance styles. Tobacco extract is the most important component of tobacco flavor and fragrance, and mainly comprises the following components: tobacco essential oil, tobacco absolute, tobacco extract, tobacco tincture, supercritical (sub-) fluid tobacco extract, tobacco non-enzymatic browning product, tobacco thermal processing product, tobacco unconcentrated extract, etc. The mandatory national standard of GB 41700-2022 electronic cigarette clearly specifies that the characteristic flavor of the product should not be rendered other than tobacco, and clearly requires that: the aerosol should contain nicotine and no nicotine e-cigarette product should not be marketed, 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.
The tobacco extract is mainly aimed at the extraction method or the acquisition of single components, on the one hand, the extraction material quantity is poor, the separation is needed further, and the high Nicotine content increases the flavoring difficulty, on the other hand, the environmental pollution and the waste of tobacco resources are easy to cause.
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;
step b), carrying out ultrasonic washing on the tobacco powder with deionized water for 1-3 times, and sequentially carrying out filtration and centrifugal dehydration after each ultrasonic washing to obtain washing residues;
step c), drying the water washing residues to obtain low-nicotine tobacco powder;
step d), performing carbon dioxide supercritical extraction on the low-nicotine tobacco powder once to obtain a primary extract;
step e), carrying out secondary carbon dioxide supercritical extraction on the residue after 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;
step 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 40-60 ℃ and crushed to 20-40 meshes, so as to obtain tobacco powder.
Further, in the step b), in each ultrasonic water washing, the mass ratio of deionized water to 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 primary supercritical carbon dioxide extraction conditions 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 for the secondary supercritical carbon dioxide extraction in the 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.
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 prepared according to the method of any one of the above.
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 is characterized in that deionized water is used for carrying out ultrasonic washing treatment for 1-3 times in advance on tobacco raw materials, so that nicotine and partial macromolecular impurities in tobacco powder can be dissolved, and nonpolar aroma 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 is lower than 0.5% after primary ultrasonic water washing, lower than 0.1% after secondary ultrasonic water washing, and lower than 0.05% after three ultrasonic water washing.
2. The method provided by the invention carries out ultrasonic washing treatment on the tobacco raw material in advance, can also loosen the structure of the treated tobacco powder, and is more beneficial to improving supercritical CO 2 Extraction yield of endogenous aroma components by the fluid.
3. After the primary carbon dioxide supercritical extraction is carried out, the residue is subjected to secondary supercritical extraction at a higher temperature, the degradation speed of the fragrance precursor can be accelerated by increasing the temperature, some micromolecular aldehyde ketone and ester fragrance substances are generated, the temperature is continuously increased, the Maillard reaction is accelerated, the content of Maillard reactants such as furanone, pyrone and pyrrole substances is rapidly increased, thereby not only compensating the loss of water-soluble aldehyde ketone compounds caused by ultrasonic water washing, but also generating more fragrance component substances, enriching fragrance, enabling the prepared fragrance to present more outstanding sweet taste on taste sense, improving the sweet feel of cigarette smoke and highlighting the taste characteristics of cigarette sweet and moist;
in conclusion, the preparation method of the tobacco extract provided by the invention enables the endogenous aroma components of the tobacco and the nicotine to be separated, the aroma components of the tobacco are not damaged, the nicotine content in the extract is extremely low, the aroma and taste components are 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 foregoing and other objects, features and advantages of the invention will be apparent from the following more particular descriptions of exemplary embodiments of the invention as illustrated in the accompanying drawings wherein like reference numbers generally represent like parts throughout the exemplary embodiments of the invention.
FIG. 1 is a GC/MS diagram of extract 0, extract 1 and extract 2 of example 1 of the present invention;
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the 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 or 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 in this disclosure 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 invention. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly 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;
step b), carrying out ultrasonic washing on the tobacco powder with deionized water for 1-3 times, and after each ultrasonic washing, sequentially carrying out filtration and centrifugal dehydration to obtain washing residues;
step c), drying the water washing residues to obtain low-nicotine tobacco powder;
step d), performing carbon dioxide supercritical extraction on the low-nicotine tobacco powder once to obtain a primary extract;
step e), carrying out secondary carbon dioxide supercritical extraction on the residue after 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;
step f), combining the primary extract and the secondary extract to obtain the tobacco extract.
The step a) is a step of preprocessing the tobacco raw material, and processing the tobacco raw material into a powder state so as to facilitate the subsequent procedures of water washing and supercritical extraction. The method specifically comprises the following steps: drying the tobacco raw material at 40-60 ℃ for 1-2 h, and crushing the tobacco raw material to 20-40 meshes to obtain tobacco powder. The tobacco raw material can be tobacco and tobacco products such as tobacco leaves, tobacco dust, tobacco stems and the like generated in the tobacco leaf cultivation, transportation, threshing and redrying processes and rolling processes.
Step b) is a step of ultrasonically washing the tobacco powder obtained after the pretreatment. The nicotine belongs to water-soluble components, and the main purpose of ultrasonic water washing in the step is to remove nicotine in tobacco powder, thereby reducing the content of nicotine in tobacco extract obtained by subsequent extraction. In addition, the cavitation effect generated by the ultrasound can also make the tissue of the tobacco powder more loose, which is beneficial to improving the subsequent supercriticalCO 2 Extraction yield of endogenous aroma components by the fluid.
In the step, the reason for selecting deionized water as the ultrasonic medium is as follows: on the one hand, deionized water is a polar solvent, nicotine and part of macromolecular impurities in tobacco powder can be dissolved, nonpolar aroma components are not lost, on the other hand, the tobacco powder treated by deionized water still contains a certain amount of water after being dried, and tissue cells collapse after the tobacco powder is partially removed of macromolecules such as saccharides, proteins and starch, so that the tobacco powder becomes loose, and the yield of the aroma components extracted by supercritical carbon dioxide is higher. The ultrasonic washing is carried out for 1 to 3 times in total, and the nicotine content in the washing residues is in a descending trend along with the increase of the ultrasonic washing times, but the nicotine content in the washing residues is extremely low and is generally lower than 0.05 percent after the washing times exceed 3 times; in addition, ultrasonic water washing removes nicotine and simultaneously flows water-soluble aldehyde ketone compounds and other fragrant substances; and the inventors of the present application found that as the number of water washes increases, the content of a part of the aroma compound in the extract becomes lower. In summary, the invention sets the total times of ultrasonic washing to be 1-3 times. As a preferred scheme of the embodiment, in each ultrasonic water washing, the mass ratio of deionized water to tobacco powder is (10-50): 1, the ultrasonic time is 20 min-40 min, and the ultrasonic frequency is 30 KHz-60 KHz; more preferably, the mass ratio of deionized water to tobacco powder is (25-40): 1, the ultrasonic time is 30min, and the ultrasonic frequency is 40KHz. The number of ultrasonic water washes can be selected by one skilled in the art according to particular needs.
Step c) is a process of further drying the water washing residues subjected to ultrasonic water washing and dehydration treatment, and the drying function is as follows: the water-washed tobacco powder 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 supercritical carbon dioxide and the material is affected, the material is easily agglomerated, the extraction time is prolonged, and the extraction yield is reduced. The inventor of the application finds that the water content of the tobacco powder subjected to ultrasonic water washing has an effect on supercritical extraction, when the water content of the material is higher than 15%, the extraction yield is obviously reduced, the extract has a water layer, and the quantity of partial aroma components is reduced. Further, 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 procedure is preferably as follows: and drying the water washing residues at 40-60 ℃ until the water content is 10% -15%, thus obtaining the low-nicotine tobacco powder.
Step d) performing a first carbon dioxide supercritical extraction on the low-nicotine tobacco powder obtained by drying, wherein the carbon dioxide supercritical extraction is not used 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; in addition, the low-temperature extraction can be realized, and the thermosensitive aroma components can be extracted. In the embodiment, alcohols, acids, esters, aldehyde ketones, alkanes and other substances in the low-nicotine tobacco powder can be extracted by performing one-time supercritical extraction. After one supercritical extraction, the materials in the separation kettle are desolventized, and then the primary extract is obtained. Preferably, the conditions for the first supercritical carbon dioxide extraction in this step are as follows: the extraction temperature is 40-60 ℃, the extraction pressure is 10-30 MPa, and the extraction time is 1-3 h. More preferably, the extraction temperature is 45 ℃, the extraction pressure is 30MPa, and the extraction time is 1.5-2 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 capability on polar strong and weak aroma components, has a boiling point of 78.3 ℃, is nontoxic, and is a cigarette flavoring permission solvent. Further, 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 being introduced into the carbon dioxide fluid and mixed with the low nicotine tobacco powder, and can also be introduced into the extraction kettle together with the carbon dioxide fluid.
The step e) is a step of continuously performing the secondary supercritical carbon dioxide extraction on the residue after the primary extraction. Although the supercritical water washing in the step a) is favorable for removing nicotine, part of water-soluble aldehyde ketone compounds in the tobacco powder are also lost together with the ultrasonic water washing, and in order to compensate the loss of the compounds, the step is carried out for the second supercritical extraction, and compared with the first supercritical extraction, the extraction temperature is higher, the temperature is 80-100 ℃, and the pressure is 20-30 MPa. The tobacco has complex and various flavor substances and precursor species thereof, the degradation speed of the flavor precursor can be accelerated by increasing the temperature, some micromolecular aldehyde ketone and ester flavor substances are generated, the Maillard reaction is accelerated by continuously increasing the temperature, 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 washing can be compensated, more flavor component substances are generated, and the flavor is enriched. In this step, the conditions for the secondary supercritical carbon dioxide extraction are as follows: the extraction temperature is 80-100 ℃, the extraction pressure is 20-30 MPa, and the extraction time is 1-2 h. In this step, the extraction temperature has an influence on the composition of the aroma components, and is too low, the aroma components are less in content, and too high, so that a burnt bitter component is generated, and the extraction temperature is more preferably 95-100 ℃, and most preferably 95 ℃; the extraction pressure is most preferably 30MPa. Similar to the primary supercritical extraction, absolute ethanol is also preferred as an entrainer for this step. Further, the weight-volume ratio of the low-nicotine tobacco powder to the absolute ethyl alcohol is 1g (0.05 mL-0.125 mL).
And f) after the secondary supercritical extraction, desolventizing the feed liquid in the separation kettle to obtain a secondary extract, and combining the primary extract and the secondary extract according to the step f) to obtain the tobacco extract, wherein the tobacco extract has low nicotine content and high 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 is characterized in that deionized water is used for carrying out ultrasonic washing treatment for 1-3 times in advance on tobacco raw materials, so that nicotine and partial macromolecular impurities in tobacco powder can be dissolved, and nonpolar aroma 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 is lower than 0.5% after primary ultrasonic water washing, lower than 0.1% after secondary ultrasonic water washing, and lower than 0.05% after three ultrasonic water washing.
2. The method provided by the invention carries out ultrasonic washing treatment on the tobacco raw material in advance, can also loosen the structure of the treated tobacco powder, and is more beneficial to improving supercritical CO 2 Extraction yield of endogenous aroma components by the fluid.
3. After the primary carbon dioxide supercritical extraction is carried out, the residue is subjected to secondary supercritical extraction at a higher temperature, the degradation speed of the fragrance precursor can be accelerated by increasing the temperature, some micromolecular aldehyde ketone and ester fragrance substances are generated, the temperature is continuously increased, the Maillard reaction is accelerated, the content of Maillard reactants such as furanone, pyrone and pyrrole substances is rapidly increased, thereby not only compensating the loss of water-soluble aldehyde ketone compounds caused by ultrasonic water washing, but also generating more fragrance component substances, enriching fragrance, enabling the prepared fragrance to present more outstanding sweet taste on taste sense, improving the sweet feel of cigarette smoke and highlighting the taste characteristics of cigarette sweet and moist;
in conclusion, the preparation method of the tobacco extract provided by the invention enables the endogenous aroma components of the tobacco and the nicotine to be separated, the aroma components of the tobacco are not damaged, the nicotine content in the extract is extremely low, the aroma and taste components are 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 described below with reference to specific examples:
EXAMPLE 1 Effect of the number of ultrasonic Water washes on Low temperature supercritical extraction
1. Collecting tobacco powder produced in the rolling process, drying the tobacco powder at 40 ℃ for 1h, crushing and sieving the crushed tobacco powder with a 20-mesh sieve for standby;
2. weighing 1kg of tobacco powder, loading into a flask, adding 25 times of deionized water, carrying out ultrasonic treatment at a frequency of 40KHz for 30min at normal temperature, filtering, collecting first filtrate, and centrifugally dehydrating the tobacco powder to obtain first residue; weighing 600g of first residue, adding 25 times of deionized water, carrying out ultrasonic treatment for 30min, filtering, collecting second filtrate, and centrifuging and dehydrating tobacco powder to obtain second residue; adding 25 times of deionized water into 300g of the second residue, carrying out ultrasonic treatment for 30min, filtering, collecting third filtrate, and centrifuging and dehydrating the tobacco powder to obtain third residue.
3. 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 percent;
4. 200g of dried first low-nicotine tobacco powder is weighed and put into an extraction kettle, 50mL of absolute ethyl alcohol is added, the extraction pressure is set to be 30MPa, the temperature is 45 ℃, and CO is introduced 2 The method comprises the steps of carrying out a first treatment on the surface of the Pressurizing to set pressure, circularly extracting for 1.5h, and collecting supercritical CO of tobacco 2 An extract. Since this example only analyzed the effect of ultrasonic water washing times on the low temperature carbon dioxide supercritical extraction effect, this example did not proceed with the step of secondary carbon dioxide supercritical extraction.
Sequentially carrying out CO 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 Extracting with supercritical fluid to obtain corresponding supercritical CO 2 Tobacco extract. Supercritical CO from the raw tobacco powder, the first low nicotine tobacco powder, the second low nicotine tobacco powder and the third low nicotine tobacco powder 2 The tobacco extracts are labeled as extract 0, extract 1, extract 2 and extract 3 in that order.
Taking the tobacco extract with the same amount, adding 100 mu L of 10mg/mL ethyl salicylate as an internal standard, fixing the volume to 5mL, taking a proper amount of solution, slightly filtering, and performing GC/MS analysis, wherein the result is shown in figure 1 (because figure 1 mainly shows the change of nicotine content in each extract, but the nicotine content of the extract after two ultrasonic water washes is very low, the GC/MS diagram of the extract after three ultrasonic water washes is not shown in figure 1)
The results of comparing the rates of change of the aroma components in extract 0, extract 1, extract 2 and extract 3 were analyzed with the relative amounts of the aroma components in extract 0 as reference 1 are shown in Table 1.
TABLE 1 comparison of aroma components in tobacco extracts (times)
As can be seen from table 1:
1) Part of water-soluble flavor components (because the raw materials adopt the crushing in the cigarette production process, the flavor components such as propylene glycol, glycerol and some aldehyde ketone are introduced during flavoring) are lost after one-time water washing, and basically no detection is made;
2) A small part of components such as small molecule benzoic acid, phenylacetic acid, solanone, scopoletin and the like are not affected by water washing treatment basically;
3) The content of the endogenous aroma components of most tobacco is improved to different degrees after primary, secondary and tertiary ultrasonic water washing;
4) The content of endogenous aroma components of part of tobacco is obviously improved after primary water washing; for example: beta-damascenone, geranylacetone, 4,7, 9-megastigmatrien-3-one, neophytadiene, palmitic acid, methyl palmitate, benzyl benzoate, methyl linolenate, phytol, pentadecanoic acid, stearic acid, higher alkane, squalene, vitamin E and the like are increased by more than 2 times, especially megastigmatrienone, also called tobacco ketone, which presents lasting sweet tobacco fragrance, is an important component of natural fragrance of flue-cured tobacco, can play a role in flavoring and seasoning after a small amount of the components are added into cigarettes, and the content of the components is increased by more than 3 times after one-time water washing treatment; beta-damascenone is also an extremely important aroma component in tobacco, can sweet and mellow smoke, improves bad gas, increases natural feel and sense of thickness, and increases the content by about 3 times after one-time water washing treatment; the total amount of fatty acid esters with equal chain length 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 the cigarettes with faint scent and soft smoke, and increase the faint scent and the fragrance of the cigarettes; the higher alkane is a main component of the wax of the tobacco leaf, can inhibit the loss of moisture, plays a role in moisture retention, and the content of the higher alkane is obviously increased after water washing; squalene with a reducing effect increases the content of squalene by about 5 times after one water washing; the vitamin E can reduce the damage of harmful components in the smoke to DNA, and the extraction amount is greatly increased after water washing;
5) The nicotine content is reduced by about 90%, 97% and 99% after the primary, secondary and tertiary ultrasonic water washing.
The present example is for explaining the effect of water washing and the number of times of water washing on the aroma components of carbon dioxide supercritical extraction tobacco powder, the extract is separated, the secondary supercritical extraction step is carried out on the basis of the step, the tobacco powder after primary supercritical extraction is continuously extracted after the temperature is raised, and the obtained extracts are combined to obtain the tobacco extract of the present invention, therefore, the present example does not include the secondary supercritical step, but does not influence the explanation of the water washing effect.
EXAMPLE 2 Effect of temperature of high temperature supercritical extraction on extraction Effect
1. Drying tobacco leaf raw materials in a 60 ℃ oven for 2 hours, wherein the water content is about 10%, and then crushing the tobacco leaf raw materials into tobacco powder with 20 meshes for later use;
2. 200g of dried tobacco residue is weighed and put into an extraction kettle, 50mL of absolute ethyl alcohol is added, the extraction pressure is set to be 30MPa, the temperature is 45 ℃, and CO is introduced 2 Pressurizing to set pressure, circularly extracting for 2h, decompressing and desolventizing the residue in the extraction kettle, and continuously introducing CO 2 And 20mL of absolute ethyl alcohol, continuously performing secondary supercritical extraction for 1h at 100 ℃ and 30MPa, and collecting to obtain supercritical CO 2 Tobacco extract, labeled extract G.
3. The above steps are repeated except that the temperature of the secondary supercritical extraction is 35 ℃, 45 ℃, 55 ℃, 65 ℃, 75 ℃ and 85 ℃ respectively, and the collected supercritical CO is obtained 2 The tobacco extracts are respectively marked as extract A, extract B, extract C and extractExtract D, extract E, extract F.
Equal amounts of the above extracts were taken respectively, 100. Mu.L of 10mg/mL ethyl salicylate was added as an internal standard, absolute ethanol was set to 5mL, GC/MS analysis was performed after microfiltration, and the contents of various aroma substances in the extracts were as shown in Table 2.
The results of analyzing and comparing the rate of change of the content of each kind of aroma substances in the extracts B to G with the relative content of each aroma component in the extract A as a reference 1 are shown in Table 3.
Table 2 content of various aroma substances (mg) in extract
Table 3 comparison of the content of aroma components in the extracts
As can be seen from tables 2 and 3: the total amount of furan, pyran cyclic aldehyde ketone compound in the extract starts to increase significantly at 85 ℃ to 260% at 100 ℃, wherein the 3, 5-dihydroxy-2-methyl-4H-pyran-4-one increases by 230%,2, 3-dihydro-3, 5-dihydroxy-6-methyl-4 (H) -pyran-4-one (DDMP), the extraction amount of which increases by about 7 times from 80 to 100 ℃. The ketone substances have good water solubility, show outstanding sweet taste on taste sense, can promote the sweet taste of cigarette smoke, and show the characteristics of sweet and moist taste. The extraction amount of main aroma substances in tobacco, such as solanone, geranylacetone, farnesylacetone, megastigmatrienone, 4-hydroxy-beta-dihydro-damascenone, 1-hydroxy-4-ketone-2-ionone and the like, at 80-100 ℃ is also improved by 30-100%.
It should be noted that, in this embodiment, the influence of the secondary supercritical extraction temperature on the extraction effect is verified, and in order to simplify the experimental procedure, the step of ultrasonic washing is omitted, but the influence trend of the secondary supercritical extraction temperature on the extraction effect is not affected.
EXAMPLE 3 Effect of the moisture content of the Pre-extraction Material on supercritical extraction
1. Collecting tobacco powder produced in the rolling process, adding 35 times of deionized water, carrying out ultrasonic treatment at the frequency of 40KHz for 30min at normal temperature, filtering, collecting first filtrate, and centrifugally dehydrating the tobacco powder to obtain tobacco powder residue;
2. the residue of the tobacco powder after water washing is put into a baking oven at 60 ℃ to be dried respectively until the moisture content is about 5 percent, 10 percent, 15 percent and 20 percent of the tobacco powder is reserved;
3. 200g of tobacco residue with water content of about 5% is weighed and put into an extraction kettle, the extraction pressure is set to be 30MPa, the temperature is 45 ℃, and CO is introduced 2 Pressurizing to set pressure, circularly extracting for 2h, and collecting to obtain supercritical CO 2 The tobacco extract is denoted as extract I, and the residue of tobacco dust containing about 10%,15% and 20% of water is extracted sequentially in the same way, and is respectively denoted as extract II, extract III and extract IV.
GC/MS analysis was performed on the above extract as in example 2, and the relative amounts of the various flavoring substances in the extract are shown in Table 4.
Table 4 amounts of various aroma substances (mg) in extracts
| Extract I | Extract II | Extract III | Extract IV | |
| Water content | 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 | 0.65 | 0.66 | 0.85 | 0.84 |
| Aldehyde ketones | 0.27 | 0.38 | 0.59 | 0.57 |
| Heterocyclic ring | 1.03 | 3.32 | 3.66 | 5.47 |
| Alkanes and alkanes | 4.44 | 2.72 | 2.78 | 2.71 |
| Terpenes | 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 |
As can be seen from table 4: after the tobacco powder is dried, the total extraction amount of the fragrant substances is low, and the contents of alcohols with low boiling point, small molecular acids, aldehyde ketone and the like are obviously reduced. Along with the increase of the water content, the extraction yield of the spice and the quantity of the aroma compounds are also increased, and the extraction quantity is increased to the greatest extent, and is esters, especially dihydro-actinolide, DL-pantolactone, scopoletin and the like; 2, 3-dihydro-3, 5-dihydroxy-6-methyl-4 (H) -pyran-4-one (DMPP), methylcyclopentenolone (MCP), 5-hydroxymethylfurfural and the like having a sweet smell increase with increasing moisture content of tobacco dust; terpenoids such as neophytadiene and squalene gradually decrease with increasing water content. Therefore, the material contains a proper amount of water, which can improve the performance of the supercritical fluid and is beneficial to improving the solubility of polar hydrophilic flavor substances, but when the water content is too high, the material in the extraction kettle is wet and is easy to be agglomerated under high pressure, so that the extraction yield of part of flavor components is reduced.
It should be noted that, this embodiment is used to verify the effect of the water content of the material before extraction on the supercritical extraction, so although the steps of ultrasonic washing and high-temperature supercritical extraction are omitted, the trend of the water content of the material before extraction on the supercritical extraction is not affected.
Example 4
1. Collecting tobacco powder produced in the rolling process, drying the tobacco powder at 40 ℃ for 1h, crushing and sieving the crushed tobacco powder with a 20-mesh sieve for standby;
2. weighing 1kg of tobacco powder, loading into a flask, adding 40 times of deionized water, carrying out ultrasonic treatment at the frequency of 40KHz for 30min at normal temperature, filtering, collecting filtrate, and centrifuging the tobacco powder to obtain tobacco powder residue; further drying the residue at 60deg.C to obtain tobacco powder with water content of about 15%;
3. 200g of the treated tobacco powder is weighed and put into an extraction kettle, 50mL of absolute ethyl alcohol is added, the extraction pressure is set to be 30MPa, the temperature is 45 ℃, and CO is introduced 2 Pressurizing to set pressure, circularly extracting for 1.5 hr, decompressing and desolventizing the residue in the extracting kettle, heating to 95 deg.C, introducing 20mL absolute alcohol and CO 2 Continuously performing secondary supercritical extraction under 30MPa for 1.5h, and mixing and collecting to obtain tobacco powder supercritical CO 2 An extract.
4. CO is carried out on the raw tobacco powder which is not subjected to ultrasonic water washing according to the method 2 Supercritical extraction to obtain corresponding supercritical fluidBoundary CO 2 Tobacco extract. The supercritical CO of the original tobacco powder and the tobacco powder after one-time washing 2 The tobacco extracts are in turn labeled as extract X, extract Y.
0.1g of the extract X and the extract Y are taken, 100 mu L of 10mg/mL ethyl salicylate is respectively added as an internal standard, absolute ethyl alcohol is fixed to 5mL, and a proper amount of solution is taken to pass through a 0.45 mu m organic phase filter membrane for GC/MS analysis. The relative amounts of the respective aroma components in extract X and extract Y are shown in Table 5.
Table 5 content of some aroma components (mg) in extract
Table 5 shows that: the tobacco powder is subjected to primary supercritical extraction at low temperature after primary water washing, the temperature of the extracted material is increased, and secondary supercritical extraction is continuously carried out, so that compared with the original control tobacco powder extract, the content of endogenous aroma substances in tobacco can be obviously improved, and the quantity of aldehyde ketone aroma substances is increased.
Observing the appearance, wherein the extract X has uniform color and luster and orange color; the aroma and smell evaluation shows that the cured tobacco aroma, the fresh sweet aroma and the baking aroma of the extract X are prominent, and the tobacco aroma is purer and natural.
The organic combination of different aroma components forms the aroma characteristics of the spice, so the tobacco source spice with strong applicability can be prepared by adjusting the washing times and the extraction conditions in a certain range and combining with the perfuming test result according to the nicotine content condition of the tobacco powder, and the aroma mixing and self-guaranteeing capability of the essence spice of the boosted cigarette can be improved.
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or 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 various embodiments described. The terminology used herein was chosen in order to best explain the principles of the embodiments, the practical application, or the improvement of 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 of preparing a tobacco extract, comprising:
step a), drying and crushing tobacco raw materials to obtain tobacco powder;
step b), carrying out ultrasonic washing on the tobacco powder with deionized water for 1-3 times, and sequentially carrying out filtration and centrifugal dehydration after each ultrasonic washing to obtain washing residues;
step c), drying the water washing residues to obtain low-nicotine tobacco powder;
step d), performing carbon dioxide supercritical extraction on the low-nicotine tobacco powder once to obtain a primary extract;
step e), carrying out secondary carbon dioxide supercritical extraction on the residue after the primary carbon dioxide supercritical extraction to obtain a secondary extract; the temperature of the secondary supercritical carbon dioxide extraction is 80-100 ℃ and the pressure is 20-30 MPa;
step f), combining the primary extract and the secondary extract to obtain the tobacco extract.
2. The 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 mesh, to obtain tobacco powder.
3. The method according to claim 1, wherein in the step b), the mass ratio of deionized water to 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. The method according to claim 1, wherein in step c), the water content of the low nicotine tobacco powder is between 10% and 15%.
5. The process according to claim 1, wherein the primary supercritical carbon dioxide extraction conditions in step d) are as follows:
the extraction temperature is 40-60 ℃, the extraction pressure is 10-30 MPa, the cyclic extraction is carried out, and the extraction time is 1 h-3 h.
6. The process according to claim 5, wherein in step d), absolute ethanol is used as entrainer during the extraction; 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 process according to claim 1, wherein the conditions for 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, the cyclic extraction is carried out, and the extraction time is 1 h-2 h.
8. The method according to claim 7, wherein in step e), absolute ethanol is used as entrainer during 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101491618A (en) * | 2007-04-18 | 2009-07-29 | 北京和润创新医药科技发展有限公司 | Method for separating tobacco total alkaloid from extract liquid of tobacco leftovers |
| 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 |
| CN103478892A (en) * | 2013-09-18 | 2014-01-01 | 浙江中烟工业有限责任公司 | Intrinsic tobacco aroma substance directionally and compositely extracted from tobacco raw material by water extraction method and ethanol extraction method |
| CN107660812A (en) * | 2016-07-27 | 2018-02-06 | 湖南中烟工业有限责任公司 | A kind of Flue-cured Tobacco alkali extract and extraction process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101491618A (en) * | 2007-04-18 | 2009-07-29 | 北京和润创新医药科技发展有限公司 | Method for separating tobacco total alkaloid from extract liquid of tobacco leftovers |
| 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 |
| CN103478892A (en) * | 2013-09-18 | 2014-01-01 | 浙江中烟工业有限责任公司 | Intrinsic tobacco aroma substance directionally and compositely extracted from tobacco raw material by water extraction method and ethanol extraction method |
| CN107660812A (en) * | 2016-07-27 | 2018-02-06 | 湖南中烟工业有限责任公司 | A kind of Flue-cured Tobacco alkali extract and extraction process |
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