CN115088861A - Method for preparing tobacco leaf extract by using waste tobacco leaves/tobacco powder - Google Patents
Method for preparing tobacco leaf extract by using waste tobacco leaves/tobacco powder Download PDFInfo
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- CN115088861A CN115088861A CN202210829281.6A CN202210829281A CN115088861A CN 115088861 A CN115088861 A CN 115088861A CN 202210829281 A CN202210829281 A CN 202210829281A CN 115088861 A CN115088861 A CN 115088861A
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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
- A24B15/243—Nicotine
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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
Abstract
The invention discloses a method for preparing a tobacco leaf extract by utilizing waste tobacco leaves/tobacco powder, which comprises the following steps: liquefying waste tobacco leaves/tobacco powder by near-critical water, adding a waste tobacco leaf/tobacco powder sample and distilled water into a reaction kettle according to a preset proportion, sealing the reaction kettle, heating the reaction kettle to a target temperature according to a preset heating rate, preserving heat for a preset time, naturally cooling to room temperature, discharging, filtering or centrifugally separating to obtain a solid phase and a liquid phase, and collecting gas generated in the reaction process; analyzing the components of the waste tobacco leaves/tobacco powder extract, extracting the obtained solid-phase residue by using an organic solvent, filtering, washing filter residues, drying to constant weight, concentrating and extracting the filtrate, and analyzing the components of the waste tobacco leaves/tobacco powder extract by adopting GC-MS (gas chromatography-Mass spectrometer). The invention relates to a method for preparing a tobacco leaf extract by utilizing waste tobacco leaves/tobacco powder, which utilizes a near-critical water technology and only utilizes the waste tobacco leaves/tobacco powder and water as raw materials to prepare the waste tobacco leaves/tobacco powder extract.
Description
Technical Field
The invention relates to the technical field of tobacco processing, in particular to a method for preparing a tobacco leaf extract by utilizing waste tobacco leaves/tobacco powder.
Background
In recent years, the tobacco yield in China is huge, the average tobacco yield in 2015-2019 years is about 240 ten thousand tons, and a large amount of waste tobacco leaves such as tobacco leftover leaves and tobacco dust and inventory tobacco leaves with low quality are generated every year. The waste tobacco leaves are rich in organic matters such as lignin and cellulose, and are very good biomass resources. At present, the utilization rate of the waste tobacco leaves is low, so that not only is the waste of resources caused, but also the environment is polluted if the waste tobacco leaves are not treated properly.
In recent years, resource utilization of waste biomass has been studied more and more, and the following issues are mainly focused: firstly, the tobacco sheets are prepared by utilizing waste such as waste tobacco leaves/tobacco powder, tobacco flakes and the like through a rolling method, a thick liquid method, a paper making method and the like, the tobacco sheets also play an important role in the aspects of reducing the tar content of cigarettes, reducing the harm of the cigarettes, improving the quality of the cigarettes and the like, but the waste tobacco leaves/tobacco powder for preparing the tobacco sheets is very limited, and most of the waste tobacco leaves/tobacco powder is discarded and treated. Secondly, the waste tobacco leaves/tobacco powder not only contain abundant carbon sources and nitrogen sources such as saccharides and proteins, but also have a loose structure and are ideal microbial solid fermentation beds, so that many experts and scholars study the application of different types of microbes to the waste tobacco leaves/tobacco powder solid fermentation beds, the direct fermentation of the waste tobacco leaves/tobacco powder is difficult to thoroughly eliminate pathogenic microbes and nicotine, and volatile components in the waste tobacco leaves/tobacco powder are not beneficial to microbial fermentation. Thirdly, extracting natural components, namely extracting nicotine, solanesol, vegetable protein, pectin and the like by using waste tobacco leaves/tobacco powder as raw materials through an extraction technology, wherein the existing technology for extracting nicotine from the tobacco leaves or the waste tobacco leaves/tobacco powder is complex and has high production difficulty; the solanesol is extracted by adopting an organic solvent, and after a crude product is obtained, the solanesol is purified by methods such as dewaxing, saponification, crystallization, recrystallization and the like, so that the operation is complicated, the cost is high, and the industrial production is difficult; the plant protein is extracted from the solid phase part after acidification, the treatment is complicated, and the environment is polluted. Pectin can be extracted by a boiling water extraction method, an acid hydrolysis method, a microbiological method (enzyme separation method) and an ion exchange resin method, but the extraction efficiency is not high and the purification is difficult at present. In a word, the separation of specific chemical components from the tobacco leaves is difficult to realize large-scale production, a large amount of organic solvents are needed in the extraction and preparation processes of the compounds, the time and the labor are consumed, the secondary pollution is caused to the environment, and meanwhile, the solid phase part after extraction is not further processed and utilized, so that the waste of resources is caused.
Therefore, a method for preparing a tobacco leaf extract using waste tobacco leaves/tobacco powder is needed.
Disclosure of Invention
The invention aims to provide a method for preparing a tobacco leaf extract by utilizing waste tobacco leaves/tobacco powder, which aims to solve the problems in the prior art and can prepare the waste tobacco leaves/tobacco powder extract by only utilizing the waste tobacco leaves/tobacco powder and water as raw materials.
The invention provides a method for preparing a tobacco leaf extract by utilizing waste tobacco leaves/tobacco powder, which comprises the following steps:
liquefying waste tobacco leaves/tobacco powder by near-critical water, adding a waste tobacco leaf/tobacco powder sample and distilled water into a reaction kettle according to a preset proportion, sealing the reaction kettle, heating the reaction kettle to a target temperature according to a preset heating rate, preserving heat for a preset time, naturally cooling to room temperature, discharging, obtaining a solid phase and a liquid phase through filtration or centrifugal separation, and collecting gas generated in the reaction process;
analyzing the components of the waste tobacco leaves/tobacco powder extract, extracting the obtained solid-phase residue by using an organic solvent, filtering, washing filter residues, drying to constant weight, concentrating and extracting the filtrate, and analyzing the components of the waste tobacco leaves/tobacco powder extract by adopting GC-MS (gas chromatography-Mass spectrometer).
The method for preparing a tobacco leaf extract using the waste tobacco leaves/tobacco powder as described above, wherein, preferably, in the step of liquefying the waste tobacco leaves/tobacco powder with the near-critical water, the mixing ratio of the waste tobacco leaves/tobacco powder sample and the distilled water is 1:2 to 1: 20.
The method for preparing the tobacco leaf extract from the waste tobacco leaves/tobacco powder as described above, wherein, preferably, in the step of liquefying the waste tobacco leaves/tobacco powder with the near-critical water, the waste tobacco leaves/tobacco powder sample and distilled water are added into the reaction kettle according to a preset proportion, and then the total volume of the materials accounts for 1:3-3:4 of the volume of the reaction kettle.
The method for preparing the tobacco leaf extract using the waste tobacco leaves/tobacco powder as described above, wherein, preferably, in the step of liquefying the waste tobacco leaves/tobacco powder with the near-critical water, the temperature rising rate of the reaction kettle is 8 ℃/min to 15 ℃/min.
The method for preparing the tobacco leaf extract using the waste tobacco leaves/tobacco powder as described above, wherein, in the step of liquefying the waste tobacco leaves/tobacco powder using the near-critical water, it is preferable that the target temperature of the reaction kettle is 160 ℃ to 260 ℃, the steam pressure corresponding to the target temperature is 0.5MPa to 6.0MPa, and the holding time at the target temperature is 5min to 20 min.
In the method for preparing a tobacco leaf extract using waste tobacco leaves/tobacco powder as described above, it is preferable that, in the step of liquefying the waste tobacco leaves/tobacco powder with the near-critical water, the controller heating switch is turned off after the temperature is maintained for a preset time, so as to be naturally cooled to room temperature.
The method for preparing a tobacco leaf extract using waste tobacco leaves/tobacco powder as described above, wherein, preferably, in the step of liquefying the waste tobacco leaves/tobacco powder with the near-critical water, the collecting gas generated during the reaction process includes:
collecting gas generated in the reaction process through a gas sampling bag connected with a needle valve on a reaction kettle cover, weighing the gas sampling bag on an electronic balance respectively before and after collecting the gas, and recording the mass as m 0 (Kg) and m 1 (Kg), the gas yield was obtained by the subtraction method,
m qi (Qi) ＝m 1 -m 0 (1)
Wherein M represents the mass (Kg) of the waste tobacco leaves/tobacco powder raw material.
The method for preparing a tobacco leaf extract using the waste tobacco leaves/tobacco powder as described above, wherein, in the step of analyzing the components of the waste tobacco leaves/tobacco powder extract, the time for extracting the obtained solid phase residue with the organic solvent is preferably 2h to 12 h.
The method for preparing a tobacco leaf extract using the waste tobacco leaves/tobacco powder as described above, wherein, preferably, in the step of analyzing the components of the waste tobacco leaves/tobacco powder extract, after the residue is washed and dried to a constant weight, the residue rate and the conversion rate are calculated,
wherein M represents the mass (Kg) of the waste tobacco leaves/tobacco powder raw materials, M Residue of rice The mass (Kg) of the solid phase residue after drying is shown.
In the method for preparing a tobacco leaf extract from waste tobacco leaves/tobacco powder as described above, preferably, in the step of analyzing the components of the waste tobacco leaves/tobacco powder extract, after the filtrate is concentrated by a rotary evaporator, the filtrate is extracted by ethyl acetate, chloroform and n-hexane respectively, the components of the waste tobacco leaves/tobacco powder extract obtained by different treatment methods are analyzed by GC-MS,
the extract obtained by n-hexane extraction comprises alkanes, alcohols and benzenes, the extract obtained by ethyl acetate extraction comprises esters, phenols and alcohols, and the extract obtained by chloroform extraction comprises pyrazine heterocyclic compounds, phenols and aldehydes and ketones.
The invention provides a method for preparing a tobacco leaf extract by utilizing waste tobacco leaves/tobacco powder, which utilizes a near-critical water technology, does not use any organic reagent, catalyst and the like, only utilizes the waste tobacco leaves/tobacco powder and water as raw materials, and prepares the waste tobacco leaves/tobacco powder extract under the conditions of acid catalysis and alkali catalysis, thereby realizing the conversion of the waste tobacco leaves/tobacco powder with low economic value into a tobacco leaf extracting solution with high added value; the method adopted by the invention has the advantages of simple conditions, short reaction time, low energy consumption, no secondary pollution in the synthesis process and environmental protection; the waste tobacco leaf/tobacco powder extract prepared by the invention effectively realizes the reutilization of waste tobacco leaf/tobacco powder resources, and provides a conversion way of waste tobacco leaf/tobacco powder resources; the waste tobacco leaves/tobacco powder extract prepared by the method contains nicotine, nicotine degradation products, esters, phenols and other substances, contains more fragrant substances, and can be used for flavoring of tobacco products, other novel tobacco products such as heating non-combustible cigarettes, electronic cigarettes and the like or flavoring of other non-tobacco related products.
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In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described with reference to the accompanying drawings, in which:
fig. 1 is a flowchart of an embodiment of a method for preparing a tobacco leaf extract using waste tobacco leaves/tobacco powder according to the present invention.
Detailed Description
Various exemplary embodiments of the present disclosure will now be described in detail with reference to the accompanying drawings. The description of the exemplary embodiments is merely illustrative and is in no way intended to limit the disclosure, its application, or uses. The present disclosure may be embodied in many different forms and is not limited to the embodiments described herein. These embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art. It should be noted that: the relative arrangement of parts and steps, the composition of materials, numerical expressions and numerical values set forth in these embodiments are to be construed as merely illustrative, and not restrictive, unless specifically stated otherwise.
As used in this disclosure, "first", "second": and the like, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that the element preceding the word comprises the element listed after the word, and does not exclude the possibility that other elements may also be included. "upper", "lower", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships may also be changed accordingly.
In the present disclosure, when a specific component is described as being located between a first component and a second component, there may or may not be intervening components between the specific component and the first component or the second component. When it is described that a specific component is connected to other components, the specific component may be directly connected to the other components without having an intervening component, or may be directly connected to the other components without having an intervening component.
All terms (including technical or scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs unless specifically defined otherwise. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate.
As shown in fig. 1, an embodiment of the present invention provides a method for preparing a tobacco extract from waste tobacco leaves/tobacco dust, which specifically includes the following steps in an actual implementation process:
and step S1, carrying out near-critical water liquefaction on the waste tobacco leaves/tobacco powder, adding a waste tobacco leaf/tobacco powder sample and distilled water into a reaction kettle according to a preset proportion, sealing the reaction kettle, heating the reaction kettle to a target temperature according to a preset heating rate, keeping the temperature for a preset time, naturally cooling to room temperature, discharging, filtering or carrying out centrifugal separation to obtain a solid phase and a liquid phase, and collecting gas generated in the reaction process.
The near critical water is that the water is heated to the boiling point (150-350 ℃) and the pressure is controlled to keep the water in a liquid state, and at the moment, the water is in a high-temperature and high-pressure liquid state. In the state of the close boundary, the dielectric constant of water is obviously reduced, and the water is converted into a nonpolar compound from a polar compound. Near-critical water is an excellent extractant because of the reduced polarity of water, which makes many otherwise water-insoluble compounds initially readily soluble in water. The method utilizes a near-critical water technology, does not use any organic reagent, catalyst and the like, only utilizes the waste tobacco leaves/tobacco powder and water as raw materials, and prepares the waste tobacco leaves/tobacco powder extract under the conditions of acid catalysis and alkali catalysis. Because organic solvent, acid-base catalyst and other substances are not used in the extraction process, the near-critical water extraction of substances is a green treatment method. The extraction process is not only green and environment-friendly and low in price, but also can be completed within several seconds to more than ten minutes. In addition, the high temperature and high pressure state of the near critical water can also cause the pyrolysis and oxidative decomposition of a plurality of different macromolecular substances.
Wherein in the step of liquefying the waste tobacco leaves/tobacco powder by the near-critical water, the mixing ratio of the waste tobacco leaves/tobacco powder sample to the distilled water is 1:2-1: 20; adding the waste tobacco leaves/tobacco powder sample and distilled water into a reaction kettle according to a preset proportion, wherein the total volume of the materials accounts for 1:3-3:4 of the volume of the reaction kettle; the heating rate of the reaction kettle is 8-15 ℃/min, such as 10 ℃/min; the target temperature of the reaction kettle is 160-260 ℃, the steam pressure corresponding to the target temperature is 0.5-6.0 MPa, and the heat preservation time at the target temperature is 5-20 min; and after the temperature is kept for the preset time, the heating switch of the controller is closed, so that the temperature is naturally cooled to the room temperature.
Further, the collecting gas generated in the reaction process comprises:
collecting gas generated in the reaction process through a gas sampling bag connected with a needle valve on the reaction kettle cover, weighing the gas sampling bag on an electronic balance respectively before and after collecting the gas, and recording the mass as m 0 (Kg) and m 1 (Kg), by subtraction, the gas yield was obtained.
m Qi (Qi) ＝m 1 -m 0 (1)
Wherein M represents the mass (Kg) of the waste tobacco leaves/tobacco powder raw material.
And step S2, analyzing the components of the waste tobacco leaves/tobacco powder extract, extracting the obtained solid phase residue with an organic solvent, filtering, washing filter residues, drying to constant weight, concentrating and extracting the filtrate, and analyzing the components of the waste tobacco leaves/tobacco powder extract by adopting a GC-MS (gas chromatography-mass spectrometry).
Wherein, in the step of analyzing the components of the waste tobacco leaves/tobacco powder extract, the organic solvent used for extracting the solid-phase residue can be acetone, and the time for extracting the obtained solid-phase residue by the organic solvent is 2h-12 h.
Further, after the filter residue is washed and dried to constant weight, the residue rate and the conversion rate are calculated,
wherein M represents the mass (Kg) of the waste tobacco leaves/tobacco powder raw materials, M Residue of rice The mass (Kg) of the solid phase residue after drying is shown.
In one embodiment of the invention, a quantity of waste tobacco leaf/tobacco powder sample and a quantity of distilled water are added to a reaction vessel, as exemplified in table 1, and the reaction vessel is closed. The temperature is raised according to the temperature rise speed of 10 ℃/min, and the reaction kettle is heated to 160-260 ℃. Under corresponding conditions, the vapor pressure of the reaction end point at different experimental temperatures is about 0.5MPa to 6.0 MPa. And keeping the constant temperature for 15min under the condition of the experimental end temperature. After the temperature is constant, the heating switch of the controller is closed, the temperature is naturally cooled to the room temperature, and the material is discharged. Then solid phase and liquid phase are obtained by filtration or centrifugal separation. The reaction conditions, the residue rate, the conversion rate and the gas yield are shown in Table 1.
TABLE 1 results of the experiment
Furthermore, after the filtrate is concentrated by a rotary evaporator, the filtrate is extracted by ethyl acetate, trichloromethane and normal hexane respectively, components of the waste tobacco leaf/tobacco powder extract obtained by different treatment modes are analyzed by GC-MS, and in order to analyze the components in the liquid phase product, the organic solvents of ethyl acetate, trichloromethane and normal hexane have a large polarity difference and a large polarity difference with near-critical water, so that the obtained liquid phase product is further extracted by the organic solvents, and the analysis of the components in the liquid phase product is facilitated.
Specifically, the extract obtained by n-hexane extraction comprises alcohols and benzenes, the extract obtained by ethyl acetate extraction comprises esters, phenols and alcohols, and the extract obtained by chloroform extraction comprises pyrazine heterocyclic compounds, phenols and aldehydes and ketones.
Taking T6 as an example, the liquid phase product obtained by T6 is extracted by organic solvents of ethyl acetate, chloroform and normal hexane in sequence, the aroma components in the waste tobacco leaves/tobacco powder extract obtained by different processing modes are analyzed, and the results are shown in Table 2 by comparing with 150 substances in Shimadzu aroma component library, after the extraction of normal hexane, ethyl acetate and chloroform, 23, 25 and 24 aroma components are respectively detected, and 39 aroma components are totally collected. The main detected fragrant substances include alcohols, esters, pyrazines, phenols and aldehydes and ketones. The n-hexane extract contains more alcohols and benzenes, the ethyl acetate extract contains more esters, phenols and alcohols, and the chloroform extract mainly contains pyrazine heterocyclic compounds, phenols and aldehydes and ketones. The waste tobacco leaves/tobacco powder extract contains nicotine, nicotine degradation products, esters, phenols and other substances and a plurality of fragrant substances, so the extract can be used for flavoring and casing of tobacco products, other novel tobacco products such as heating non-combustible cigarettes, electronic cigarettes and the like or other non-tobacco related products, and the conversion of the waste tobacco leaves/tobacco powder with low economic value into the tobacco leaf extracting solution with high added value is realized.
TABLE 2T6 results of data screening of odor component MRM of tobacco leaf samples extracted with different solvents
Note: "-" represents no detection; the retrieval database is: shimadzu Off-flavour odor analysis database, 150 compounds in total.
According to the method for preparing the tobacco leaf extract by utilizing the waste tobacco leaves/tobacco powder, provided by the embodiment of the invention, the near-critical water technology is utilized, no organic reagent, catalyst and the like are used, only the waste tobacco leaves/tobacco powder and water are used as raw materials, and the waste tobacco leaves/tobacco powder extract is prepared under the conditions of acid catalysis and alkali catalysis, so that the conversion of the waste tobacco leaves/tobacco powder with low economic value into the tobacco leaf extracting solution with high added value is realized; the method adopted by the invention has the advantages of simple conditions, short reaction time, low energy consumption, no secondary pollution in the synthesis process and environmental protection; the waste tobacco leaf/tobacco powder extract prepared by the invention effectively realizes the reutilization of waste tobacco leaf/tobacco powder resources, and provides a conversion way of waste tobacco leaf/tobacco powder resources; the waste tobacco leaves/tobacco powder extract prepared by the method contains nicotine, nicotine degradation products, esters, phenols and other substances, contains more fragrant substances, and can be used for flavoring of tobacco products, other novel tobacco products such as heating non-combustible cigarettes, electronic cigarettes and the like or flavoring of other non-tobacco related products.
Thus far, various embodiments of the present disclosure have been described in detail. Some details that are well known in the art have not been described in order to avoid obscuring the concepts of the present disclosure. Those skilled in the art can now fully appreciate how to implement the teachings disclosed herein, in view of the foregoing description.
Although some specific embodiments of the present disclosure have been described in detail by way of example, it should be understood by those skilled in the art that the foregoing examples are for purposes of illustration only and are not intended to limit the scope of the present disclosure. It will be understood by those skilled in the art that various changes may be made in the above embodiments or equivalents may be substituted for elements thereof without departing from the scope and spirit of the present disclosure. The scope of the present disclosure is defined by the appended claims.
Claims (10)
1. A method for preparing a tobacco leaf extract from waste tobacco leaves/tobacco powder is characterized by comprising the following steps:
liquefying waste tobacco leaves/tobacco powder by near-critical water, adding a waste tobacco leaf/tobacco powder sample and distilled water into a reaction kettle according to a preset proportion, sealing the reaction kettle, heating the reaction kettle to a target temperature according to a preset heating rate, preserving heat for a preset time, naturally cooling to room temperature, discharging, obtaining a solid phase and a liquid phase through filtration or centrifugal separation, and collecting gas generated in the reaction process;
analyzing the components of the waste tobacco leaves/tobacco powder extract, extracting the obtained solid-phase residue by using an organic solvent, filtering, washing filter residues, drying to constant weight, concentrating and extracting the filtrate, and analyzing the components of the waste tobacco leaves/tobacco powder extract by adopting GC-MS.
2. The method for preparing a tobacco leaf extract using the waste tobacco leaves/tobacco powder according to claim 1, wherein a mixing ratio of the waste tobacco leaves/tobacco powder sample and distilled water is 1:2 to 1:20 in the step of liquefying the waste tobacco leaves/tobacco powder with the near-critical water.
3. The method for preparing the tobacco leaf extract from the waste tobacco leaves/tobacco powder according to claim 1, wherein in the step of liquefying the waste tobacco leaves/tobacco powder with the near-critical water, after a waste tobacco leaf/tobacco powder sample and distilled water are added into a reaction kettle according to a preset proportion, the total volume of the materials accounts for 1:3-3:4 of the volume of the reaction kettle.
4. The method for preparing tobacco leaf extract using waste tobacco leaves/tobacco powder according to claim 1, wherein the temperature rising rate of the reaction vessel in the step of liquefying the waste tobacco leaves/tobacco powder using the near-critical water is 8 ℃/min to 15 ℃/min.
5. The method for preparing a tobacco leaf extract from waste tobacco leaves/tobacco powder according to claim 4, wherein in the step of liquefying the waste tobacco leaves/tobacco powder with the near-critical water, the target temperature of the reaction kettle is 160 ℃ to 260 ℃, the steam pressure corresponding to the target temperature is 0.5MPa to 6.0MPa, and the holding time at the target temperature is 5min to 20 min.
6. The method for preparing a tobacco leaf extract from waste tobacco leaves/tobacco powder according to claim 1, wherein in the step of liquefying the waste tobacco leaves/tobacco powder with the near-critical water, the controller heating switch is turned off after the temperature is maintained for a preset time, so as to be naturally cooled to room temperature.
7. The method for preparing tobacco leaf extract using waste tobacco leaves/tobacco powder according to claim 6, wherein the collecting gas generated during the reaction in the step of liquefying the waste tobacco leaves/tobacco powder with the near-critical water comprises:
collecting gas generated in the reaction process through a gas sampling bag connected with a needle valve on a reaction kettle cover, weighing the gas sampling bag on an electronic balance respectively before and after collecting the gas, and recording the mass as m 0 (Kg) and m 1 (Kg), the gas yield was obtained by the subtraction method,
m qi (Qi) ＝m 1 -m 0 (1)
Wherein M represents the mass (Kg) of the waste tobacco leaves/tobacco powder raw material.
8. The method for preparing a tobacco leaf extract from waste tobacco leaves/tobacco powder according to claim 1, wherein the time for extracting the resulting solid phase residue with an organic solvent in the step of analyzing the components of the waste tobacco leaves/tobacco powder extract is 2h to 12 h.
9. The method of preparing a tobacco leaf extract using waste tobacco leaves/tobacco powder according to claim 1, wherein in the step of analyzing the components of the waste tobacco leaves/tobacco powder extract, after the residue is washed and dried to a constant weight, the residue rate and the conversion rate are calculated,
wherein M represents the mass (Kg) of the waste tobacco leaves/tobacco powder raw materials, and M Residue of rice Represents the mass (Kg) of the solid phase residue after drying.
10. The method for preparing a tobacco leaf extract from waste tobacco leaves/tobacco powder according to claim 1, wherein in the step of analyzing the components of the waste tobacco leaves/tobacco powder extract, after the filtrate is concentrated by a rotary evaporator, the filtrate is extracted by ethyl acetate, chloroform and n-hexane respectively, and the components of the waste tobacco leaves/tobacco powder extract obtained by different treatment methods are analyzed by GC-MS,
the extract obtained by n-hexane extraction comprises alkanes, alcohols and benzenes, the extract obtained by ethyl acetate extraction comprises esters, phenols and alcohols, and the extract obtained by chloroform extraction comprises pyrazine heterocyclic compounds, phenols and aldehydes and ketones.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115669994A (en) * | 2022-10-26 | 2023-02-03 | 河南农业大学 | Method for improving near-critical water extraction tobacco leaf biomass by organic catalyst |
| CN115669993A (en) * | 2022-10-26 | 2023-02-03 | 河南农业大学 | Method for improving near-critical water extraction tobacco leaf biomass by using inorganic catalyst |
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