CN115715598A - Method for preparing tobacco organic acid by deep eutectic solvent - Google Patents
Method for preparing tobacco organic acid by deep eutectic solvent Download PDFInfo
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- CN115715598A CN115715598A CN202211523230.7A CN202211523230A CN115715598A CN 115715598 A CN115715598 A CN 115715598A CN 202211523230 A CN202211523230 A CN 202211523230A CN 115715598 A CN115715598 A CN 115715598A
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Abstract
The invention discloses a method for preparing tobacco organic acid by using a deep eutectic solvent, which comprises the following preparation steps: crushing the tobacco raw materials, putting the crushed tobacco raw materials into a microwave extraction container, adding a pretreated deep eutectic solvent for microwave-assisted extraction to obtain a tobacco organic acid primary extract, adding a volatile organic solvent into the primary extract for liquid-liquid extraction, collecting an organic solvent layer, and concentrating and enriching under reduced pressure to obtain the tobacco organic acid component. The invention effectively realizes the full extraction and enrichment of organic acid in tobacco, has better harmony on cigarettes as endogenous organic acid components of the tobacco, and has remarkable effects on improving the texture and the fineness of high-end cigarettes, reducing the irritation and enriching the herbal fragrance of the cigarette cigarettes.
Description
Technical Field
The invention relates to the technical field of tobacco chemistry, in particular to a method for preparing tobacco organic acid by using a deep eutectic solvent.
Technical Field
The organic acid is an important component of flavor components in tobaccos and tobacco products, is various in types and large in content difference and accounts for 12% -16% of the total content of dry matters in the tobaccos. Organic acids are classified into volatile organic acids and non-volatile organic acids. The volatile organic acid in tobacco is C 10 The lower fatty acid and the partial aromatic acid can directly enter smoke in the smoking process of the cigarette, and have important effects on the fragrance and the taste of the cigarette. The non-volatile organic acid in the tobacco contains malic acid, citric acid, oxalic acid and the like in a high content, and the organic acid can adjust the pH value of the tobacco and effectively promote the acid-base balance of the tobacco, so that the quality of the cigarette is improved. The organic acid in the tobacco is used as the raw material, the deep eutectic solvent is used as a medium to perform microwave-assisted rapid extraction on the organic acid in the tobacco, and then the organic solvent is used for liquid-liquid extraction to enrich and prepare the organic acid in the tobacco, so that the organic acid has higher value and significance for improving the cigarette quality for high-grade tobacco flavor.
The patent of the tobacco organic acid extraction is very rare, and part of the related patent and literature is limited to the research of the tobacco extract liquid for acid-base separation to obtain nicotine or organic acid. For example, chinese patent CN103371432B discloses a method for preparing organic acid extract of flue-cured tobacco, which comprises adjusting pH of aqueous solution, and performing acid-base separation to obtain nonvolatile organic acid component of flue-cured tobacco; CN111781286A discloses a propyl ester analysis method of organic acid substances in tobacco and tobacco products; CN103720031A discloses a method for preparing tobacco extract by adding a small amount of phosphoric acid or sulfuric acid into alcohol for extraction. These patents are not good for the enrichment of organic acid in tobacco, or the process is complicated, and the harmful solvent is more.
The patent of preparing the tobacco organic acid by adopting the deep eutectic solvent and microwave assistance and then liquid-liquid extraction is not reported, and related patents comprise: chinese patent CN114044835A discloses a method for extracting chitin from crayfish shells by microwave-assisted eutectic solvent; CN109876489A discloses a eutectic solvent combined with microwave-assisted extraction and then centrifugal separation of plants to obtain active ingredients; CN109609270A discloses a method for microwave-assisted extraction of eutectic solvent and then steam distillation extraction of essential oil in spice; CN109609271A discloses eutectic solvent microwave-assisted extraction and steam distillation for extracting essential oil from medicinal materials. Most of the patents adopt eutectic solvent microwave-assisted extraction or steam distillation and then extraction separation to obtain essential oil, and the yield is low and the method is complicated.
Disclosure of Invention
The invention aims to provide a method for preparing tobacco organic acid by using a deep eutectic solvent, aiming at overcoming the defects in the prior art. The deep eutectic solvent is used for microwave-assisted extraction, organic acid components in tobacco are effectively extracted, and the organic acid is obtained by liquid-liquid extraction and enrichment of the organic solvent, so that the tobacco organic acid has unique tobacco original fragrance and acid fragrance. The tobacco flavor enhancer can be used for high-grade cigarettes to improve the smoking texture of the cigarettes, soften smoke and strengthen comfort, and can endow the cigarettes with unique tobacco flavor and good harmony. The method widens the field of aroma enhancement and enrichment of the tobacco endogenous extract as the traditional spice and improves the thick sense, solves the problem of incongruity of the chemically synthesized monomer organic acid in the cigarette, and effectively improves the economic value of the tobacco organic acid in the cigarette.
The invention is realized by the following technical scheme, and the method for preparing the tobacco organic acid by using the deep eutectic solvent comprises the following preparation steps:
(1) Preparing raw materials: crushing the tobacco raw material for later use;
(2) Preparing a deep eutectic solvent: the hydrogen bond acceptor is one of choline chloride and betaine, the hydrogen bond donor is organic acid or a mixed system of organic acid and polyalcohol to form a binary or ternary deep eutectic solvent, and the transparent and uniform deep eutectic solvent is prepared by heating;
(3) Microwave extraction: putting tobacco raw materials into a microwave extraction container, adding a prepared deep eutectic solvent and water, and performing microwave extraction to obtain a tobacco organic acid primary extract I;
(4) Liquid-liquid extraction: and (3) adding a volatile organic solvent into the tobacco organic acid primary extract I by volume for liquid-liquid extraction, collecting an upper-layer organic solvent extraction liquid, and concentrating the extraction liquid until no solvent is distilled off to obtain the tobacco organic acid component.
Further, the tobacco raw material in the step (1) is one of burley tobacco, air-cured tobacco, sun-cured tobacco, aromatic tobacco and flue-cured tobacco.
Further, the organic acid in the step (2) is one of malic acid, citric acid, succinic acid and phenylacetic acid, so that alkaline substances such as nicotine and the like are prevented from being extracted in the extraction process, and the enrichment of the organic acid in tobacco is facilitated; the polyalcohol is one of propylene glycol, ethylene glycol and glycerol.
Furthermore, the molar ratio of the binary system of the hydrogen bond acceptor and the hydrogen bond donor in the step (2) is 1 (1-8), and the molar ratio of the ternary system is 1 (1-8) to 1-8.
Further, the transparent and uniform deep eutectic solvent in the step (2) is prepared by heating and stirring at the temperature of 50-100 ℃.
Further, the mixed system of the deep eutectic solvent and water in the step (3) has a water content of 15-50% (mass ratio).
Further, the microwave extraction conditions in the step (3) are that an extraction system with a material-liquid ratio of 1.
Further, the liquid-liquid extraction multiple of the volatile organic solvent in the step (4) is 1 to 20 times.
Further, the volatile organic solvent in the step (4) is one of petroleum ether, n-hexane, dichloromethane and chloroform.
Further, the organic acid component of the tobacco in the step (4) has unique original tobacco fragrance and rich fragrance.
The method takes tobacco as a raw material, adopts a deep eutectic solvent for microwave-assisted extraction, and performs liquid-liquid extraction through a volatile organic solvent to enrich and prepare the organic acid component of the tobacco. The innovation points and the technical effects of the invention are as follows: according to the organic acid characteristics of the tobacco raw materials, the acid deep eutectic solvent is adopted for microwave-assisted rapid extraction, so that the added acid and nicotine in the tobacco are neutralized, the tobacco organic acid extract without free nicotine is extracted, liquid-liquid extraction is carried out through the volatile organic solvent, and the tobacco organic acid component is obtained through concentration and enrichment. The process is reasonable in design, efficient and rapid, the texture of the obtained organic acid component in the high-end cigarette is effectively improved, the smoke is softened, the irritation is reduced, the unique tobacco original fragrance is given, and the quality is excellent.
Detailed Description
The following examples are intended to illustrate the present invention in further detail, but are not intended to limit the scope of the present invention. The following examples are set forth merely to aid in the understanding of the invention. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Example 1
Pulverizing Burley tobacco, and placing into microwave-assisted extraction container.
Preparing a deep eutectic solvent: choline chloride-malic acid-propylene glycol are mixed according to a molar ratio of 1.
Microwave extraction: adding 15% of water by mass into the deep eutectic solvent to form a water-containing deep eutectic solvent system, uniformly mixing the burley tobacco raw material and the water-containing deep eutectic solvent according to the ratio of material to liquid of 1.
Liquid-liquid extraction: adding 10 times volume of petroleum ether into the extract, performing oscillation extraction, collecting the upper layer of petroleum ether extract, and concentrating until no solvent is distilled off to obtain burley tobacco organic acid component with yield of 2.6%.
TABLE 1 Burley tobacco organic acid test results
The detection basis is as follows: TCJC-ZY-IV-004-2012
Example 2
Crushing sun-cured tobacco, and placing into a microwave extraction container.
Preparing a deep eutectic solvent: mixing betaine-phenylacetic acid according to a molar ratio of 1.
Microwave extraction: adding 30% of water by mass into the deep eutectic solvent to form a water-containing deep eutectic solvent system, uniformly mixing the sun-cured tobacco raw material and the water-containing deep eutectic solvent according to the ratio of material to liquid of 1.
Liquid-liquid extraction: adding 15 times volume of n-hexane into the extract liquid for oscillation extraction, collecting n-hexane layer extract liquid, concentrating until no solvent is distilled off, and obtaining the organic acid component of the sun-cured tobacco, wherein the yield is 1.8%.
TABLE 2 organic acid test results of sun-cured tobacco
The detection basis is as follows: TCJC-ZY-IV-004-2012
Example 3
And crushing the aired tobacco, and putting the aired tobacco into a microwave extraction container.
Preparing a deep eutectic solvent: the method comprises the following steps of mixing choline chloride-succinic acid-glycerol according to a molar ratio of 1.
Microwave extraction: adding 50% of water by mass into the deep eutectic solvent to form a water-containing deep eutectic solvent system, uniformly mixing the air-cured tobacco and the water-containing deep eutectic solvent according to the ratio of material to liquid of 1.
Liquid-liquid extraction: adding 1 volume of chloroform into the extract for oscillation extraction, collecting the chloroform layer extract, concentrating until no solvent is distilled off, and obtaining the organic acid component of the tobacco leaf with the yield of 1.1%.
TABLE 3 tobacco curing organic acid test results
The detection basis is as follows: TCJC-ZY-IV-004-2012
Example 4
After being crushed, the flue-cured tobacco raw material is put into a microwave extraction container.
Preparing a deep eutectic solvent: mixing betaine-citric acid-ethylene glycol according to a molar ratio of 1.
Microwave extraction: adding 25% of water by mass into the deep eutectic solvent to form a water-containing deep eutectic solvent system, uniformly mixing the flue-cured tobacco raw material and the water-containing deep eutectic solvent according to the ratio of material to liquid of 1.
Liquid-liquid extraction: adding dichloromethane with volume of 20 times of that of the extract liquor to carry out oscillation extraction, collecting dichloromethane layer extract liquor, concentrating until no solvent is distilled off, and obtaining organic acid components of the flue-cured tobacco, wherein the yield is 0.7%.
TABLE 4 organic acid test results for flue-cured tobacco
The detection basis is as follows: TCJC-ZY-IV-004-2012
It should be noted that the parameters of the embodiments described herein are only used for matching the content disclosed in the specification, so as to enable those skilled in the art to understand and read, and are not used to limit the practical limit conditions of the present invention, and any changes of the ratio or the adjustment of the components should still fall within the scope of the technical content disclosed in the present invention without affecting the efficacy and the purpose of the present invention.
Claims (10)
1. A method for preparing tobacco organic acid by using deep eutectic solvent is characterized in that: the preparation method comprises the following preparation steps:
(1) Preparing raw materials: crushing the tobacco raw material for later use;
(2) Preparing a deep eutectic solvent: the hydrogen bond acceptor is one of choline chloride and betaine, the hydrogen bond donor is organic acid or a mixed system of organic acid and polyalcohol, a binary or ternary deep eutectic solvent is formed, and the transparent and uniform deep eutectic solvent is prepared by heating;
(3) Microwave extraction: putting tobacco raw materials into a microwave extraction container, adding a prepared deep eutectic solvent and water, and performing microwave extraction to obtain a tobacco organic acid primary extract I;
(4) Liquid-liquid extraction: and (3) adding a volatile organic solvent into the tobacco organic acid primary extract I by volume for liquid-liquid extraction, collecting an upper-layer organic solvent extraction liquid, and concentrating the extraction liquid until no solvent is distilled off to obtain the tobacco organic acid component.
2. The method for preparing tobacco organic acid by using deep eutectic solvent according to claim 1, wherein: the tobacco raw material in the step (1) is one of burley tobacco, air-cured tobacco, sun-cured tobacco, aromatic tobacco and flue-cured tobacco.
3. The method for preparing tobacco organic acid by using deep eutectic solvent as claimed in claim 1, wherein: the organic acid in the step (2) is one of malic acid, citric acid, succinic acid and phenylacetic acid; the polyalcohol is one of propylene glycol, ethylene glycol and glycerol.
4. The method for preparing tobacco organic acid by using deep eutectic solvent according to claim 1, wherein: the molar ratio of the binary system of the hydrogen bond acceptor and the hydrogen bond donor in the step (2) is 1 (1-8), and the molar ratio of the ternary system is 1 (1-8) to 1-8.
5. The method for preparing tobacco organic acid by using deep eutectic solvent according to claim 1, wherein: the heating temperature in the step (2) is 50 to 100 ℃.
6. The method for preparing tobacco organic acid by using deep eutectic solvent as claimed in claim 1, wherein: the mixed system of the deep eutectic solvent and water in the step (3) has the water content of 15-50 percent (mass ratio).
7. The method for preparing tobacco organic acid by using deep eutectic solvent as claimed in claim 1, wherein: the microwave extraction conditions in the step (3) are that the material-liquid ratio is 1 to 5-30, the microwave power is 200-750W, and the extraction time is 0.5-6 h.
8. The method for preparing tobacco organic acid by using deep eutectic solvent as claimed in claim 1, wherein: the liquid-liquid extraction multiple of the volatile organic solvent in the step (4) is 1 to 20 times.
9. The method for preparing tobacco organic acid by using deep eutectic solvent as claimed in claim 1, wherein: and (4) the volatile organic solvent is one of petroleum ether, normal hexane, dichloromethane and chloroform.
10. The method for preparing tobacco organic acid by using deep eutectic solvent according to claim 1, wherein: the organic acid component of the tobacco in the step (4) has unique tobacco original fragrance and rich fragrance.
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| CN107694147A (en) * | 2017-11-02 | 2018-02-16 | 南京林业大学 | It is a kind of to be used to extract deep congruent melting solvent of five kinds of organic acids of ginkgo leaf and preparation method thereof and extracting method simultaneously |
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