CN101209985A - Method for extracting carotinoid from tobacco leaf by overcritical CO2 and application of the carotinoid in perfuming cigarette - Google Patents
Method for extracting carotinoid from tobacco leaf by overcritical CO2 and application of the carotinoid in perfuming cigarette Download PDFInfo
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- CN101209985A CN101209985A CNA2006101600041A CN200610160004A CN101209985A CN 101209985 A CN101209985 A CN 101209985A CN A2006101600041 A CNA2006101600041 A CN A2006101600041A CN 200610160004 A CN200610160004 A CN 200610160004A CN 101209985 A CN101209985 A CN 101209985A
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Abstract
The invention discloses a method for extracting carotenoid from tobacco leaves by supercritical CO2 and an application thereof in cigarette flavoring, which comprises pretreatment of the tobacco leaves raw material, extraction of the supercritical CO2 and column chromatographic separation and purification and the carotenoid is prepared. The prepared carotenoid can be used for the cigarette flavoring after oxidative degradation. The advantages of the invention are that: 1. the invention has simple technique, stable operation, high extraction efficiency which is about 30 percent than organic solvent and high purity of the prepared product (up to 90 percent or more); 2. column chromatography is directly carried out to the carotenoid extracted from the supercritical CO2 without saponification, thus not only reducing steps but also promoting the yield; 3. degradation product of the carotenoid has better flavoring effect in the cigarette, can enrich smoke gas, achieve elegant flavor and has fresh and sweet fruit flavor, and the smoking turns to be velvet; 4. the value in use of the tobacco leaves can be developed by implementing the invention, thereby promoting the utilization ratio of the tobacco leaves.
Description
Technical field
The present invention relates to a new purposes that grows tobacco and the extracting method of carotenoid, particularly a kind of supercritical CO of using
2Extract the method for carotenoid in the tobacco leaf and the application in perfuming cigarette thereof.
Background technology
At present, extracting the domestic and international widely used method of carotenoid is: extract from natural phant and salt algae with organic solvent, after being raw materials pretreatment, add certain organic solvent lixiviate several repeatedly, filter, concentrate behind the merging filtrate, obtain the carotenoid raw product, organic solvent commonly used is methyl alcohol, ethanol, sherwood oil, anhydrous diethyl ether, acetone etc.Though this method technology is simple, but quality product is not ideal, often exists carotenoid poorly soluble, and the color and luster variation waits shortcoming greatly, and the use of a large amount of organic solvents can bring pollution in various degree and be difficult for recovery in the leaching process, and it is proper to be used for experimental study.
The characteristic perfume material of tobacco mainly is its contained micro-content organism, and its effect substantially exceeds the various essence spice for cigarette that in the past used, and the fragrance thresholding of the degraded product of carotenoid is relatively low, and pungency is less, and is big to the fragrance contribution rate.Therefore, extracting the carotenoid material from tobacco is used for perfuming cigarette and is faced a difficult problem a possible approach is provided by solving present low-coke tar cigarette.Owing to reasons such as geographical environment, planting technologies, annual all have the inferior grade tobacco leaf of certain quantity can not be used for production of cigarettes, simultaneously, also inevitably produces some tankage in the production of cigarettes, use can not, hesitate to discard.How to utilize the potential value of these " refuses ", turn waste into wealth, the utilization ratio that improves tobacco leaf is to need one of problem that solves at present.
Summary of the invention
The objective of the invention is: a kind of extraction efficiency height, fast, pollution-free, the simple tobacco leaf carotenoid of the technology extracting method of speed are provided, and its carotenoid extract is applied to perfuming cigarette after further oxide treatment.
For achieving the above object, the technical solution used in the present invention is: a kind of supercritical CO of using
2Extract the method for carotenoid in the tobacco leaf and the application in perfuming cigarette thereof, comprise raw tobacco material pre-treatment, supercritical CO
2Extraction, column chromatographic isolation and purification get carotenoid, and the oxidative degradation of gained carotenoid be can be used in the perfuming cigarette.
Concrete processing step is as follows:
(1) tobacco leaf is dried under 30-60 ℃ of condition pulverizes the 20-100 mesh sieve, obtain the tobacco leaf powder;
(2) during the tobacco leaf powder that step 1 is obtained was packed extraction kettle into, adding ethanol or acetone or ethyl acetate was entrainment agent, and at extracting pressure 20-50MPa, extraction temperature 30-60 ℃, the cycling extraction through 1-4 hour obtains rough carotenoid product;
(3) the rough carotenoid product that step 2 is obtained is through alumina column chromatography, and sherwood oil, acetone carry out gradient elution, obtains refining carotenoid product;
(4) the refining carotenoid product that step 3 is obtained is made solvent, air or H with ethanol or sherwood oil or ether
2O
2Or AgNO
3Make oxygenant, reflux 6-10 hour, behind the cold filtration, obtain degraded product;
(5) the carotenoid degraded product that step 4 is obtained with ethanol or ethylene glycol or 1, behind 2-propylene glycol or the glycerine dilution finite concentration, is sprayed at and is used for perfuming cigarette on the pipe tobacco.
The perfuming of degraded product described in the step 5 concentration is 0.01-0.1%.
Advantage of the present invention is:
1. technology of the present invention is simple, stable, and the extraction efficiency height is higher by about 30% than organic solvent extraction rate, the product purity height of producing (reaching more than 90%), and purity can reach more than 98% behind further column chromatographic isolation and purification, and pollution-free.
2. supercritical CO
2The carotenoid that extracts does not need saponification, directly carries out column chromatography and separates, and has both reduced step, has improved yield again.
3. class Radix Dauci Sativae degraded product has perfuming effect preferably in cigarette, can plentiful flue gas, and make fragrance become graceful, and have fresh and sweet fruital, inhale flavor and also becomes pure and mild.
4. enforcement the present invention can develop the utility value of tobacco, improves the utilization ratio of tobacco leaf.
Description of drawings
Accompanying drawing is a process flow diagram of the present invention.
Embodiment
As shown in drawings, at first pre-treatment gets the tobacco leaf powder to raw tobacco material, then the tobacco leaf powder is put into the extraction axe and adds ethanol, carries out supercritical CO
2Extraction, the carotenoid raw product, column chromatographic isolation and purification obtains the carotenoid highly finished product then, can identify its structure with UV and IR spectrum, nuclear-magnetism.To the oxidative degradation of carotenoid highly finished product, can be used for perfuming cigarette.Below by specific embodiment implementation method of the present invention is further described, but content of the present invention be not limited to for embodiment.
Embodiment 1
Concrete processing step is as follows:
(1) tobacco leaf is dried under 30 ℃ of conditions pulverizes 20 mesh sieves, obtain the tobacco leaf powder;
(2) during the tobacco leaf powder that step 1 is obtained was packed extraction kettle into, adding ethanol was entrainment agent, and at extracting pressure 20MPa, 30 ℃ of extraction temperature through 1 hour cycling extraction, obtain rough carotenoid product;
(3) the rough carotenoid product that step 2 is obtained is through alumina column chromatography, and sherwood oil, acetone carry out gradient elution, obtains refining carotenoid product;
(4) the refining carotenoid product that step 3 is obtained is made solvent with ethanol, air oxidant, and reflux 6 hours behind the cold filtration, obtains degraded product;
(5) the carotenoid degraded product that step 4 is obtained, become 0.01% concentration with alcohol dilution after, be sprayed at and be used for perfuming cigarette on the pipe tobacco.
Embodiment 2
Concrete processing step is as follows:
(1) tobacco leaf is dried under 40 ℃ of conditions pulverizes 40 mesh sieves, obtain the tobacco leaf powder;
(2) during the tobacco leaf powder that step 1 is obtained was packed extraction kettle into, adding acetone was entrainment agent, and at extracting pressure 30MPa, 40 ℃ of extraction temperature through 2 hours cycling extraction, obtain rough carotenoid product;
(3) the rough carotenoid product that step 2 is obtained is through alumina column chromatography, and sherwood oil, acetone carry out gradient elution, obtains refining carotenoid product;
(4) the refining carotenoid product that step 3 is obtained is made solvent with sherwood oil, H
2O
2Make oxygenant, reflux 7 hours behind the cold filtration, obtains degraded product;
(5) the carotenoid degraded product that step 4 is obtained after spent glycol is diluted to 0.04% concentration, is sprayed at and is used for perfuming cigarette on the pipe tobacco.
Embodiment 3
Concrete processing step is as follows:
(1) tobacco leaf is dried under 50 ℃ of conditions pulverizes 80 mesh sieves, obtain the tobacco leaf powder;
(2) during the tobacco leaf powder that step 1 is obtained was packed extraction kettle into, the adding ethyl acetate was an entrainment agent, and at extracting pressure 40MPa, 50 ℃ of extraction temperature through 3 hours cycling extraction, obtain rough carotenoid product;
(3) the rough carotenoid product that step 2 is obtained is through alumina column chromatography, and sherwood oil, acetone carry out gradient elution, obtains refining carotenoid product;
(4) the refining carotenoid product that step 3 is obtained is made solvent with ether, AgNO
3Make oxygenant, reflux 8 hours behind the cold filtration, obtains degraded product;
(5) the carotenoid degraded product that step 4 is obtained with 1, after the 2-propylene glycol dilutes 0.06% concentration, is sprayed at and is used for perfuming cigarette on the pipe tobacco.
Embodiment 4
Concrete processing step is as follows:
(1) tobacco leaf is dried under 60 ℃ of conditions pulverizes 100 mesh sieves, obtain the tobacco leaf powder;
(2) during the tobacco leaf powder that step 1 is obtained was packed extraction kettle into, adding ethanol was entrainment agent, and at extracting pressure 50MPa, 60 ℃ of extraction temperature through 4 hours cycling extraction, obtain rough carotenoid product;
(3) the rough carotenoid product that step 2 is obtained is through alumina column chromatography, and sherwood oil, acetone carry out gradient elution, obtains refining carotenoid product;
(4) the refining carotenoid product that step 3 is obtained is made solvent with sherwood oil, air oxidant, and reflux 10 hours behind the cold filtration, obtains degraded product;
(5) the carotenoid degraded product that step 4 is obtained, dilute 0.1% concentration with glycerine after, be sprayed at and be used for perfuming cigarette on the pipe tobacco.
Claims (3)
1. use supercritical CO for one kind
2Extract the method for carotenoid in the tobacco leaf and the application in perfuming cigarette thereof, it is characterized in that: comprise raw tobacco material pre-treatment, supercritical CO
2Extraction, column chromatographic isolation and purification get carotenoid, and the oxidative degradation of gained carotenoid be can be used in the perfuming cigarette.
2. the supercritical CO of using as claimed in claim 1
2Extract the method for carotenoid in the tobacco leaf and the application in perfuming cigarette thereof, it is characterized in that concrete processing step is as follows:
(1) tobacco leaf is dried under 30-60 ℃ of condition pulverizes the 20-100 mesh sieve, obtain the tobacco leaf powder;
(2) during the tobacco leaf powder that step 1 is obtained was packed extraction kettle into, adding ethanol or acetone or ethyl acetate was entrainment agent, and at extracting pressure 20-50MPa, extraction temperature 30-60 ℃, the cycling extraction through 1-4 hour obtains rough carotenoid product;
(3) the rough carotenoid product that step 2 is obtained is through alumina column chromatography, and sherwood oil, acetone carry out gradient elution, obtains refining carotenoid product;
(4) the refining carotenoid product that step 3 is obtained is made solvent, air or H with ethanol or sherwood oil or ether
2O
2Or AgNO
3Make oxygenant, reflux 6-10 hour, behind the cold filtration, obtain degraded product;
(5) the carotenoid degraded product that step 4 is obtained with ethanol or ethylene glycol or 1, behind 2-propylene glycol or the glycerine dilution finite concentration, is sprayed at and is used for perfuming cigarette on the pipe tobacco.
3. the supercritical CO of using as claimed in claim 2
2Extract the method for carotenoid in the tobacco leaf and the application in perfuming cigarette thereof, it is characterized in that: the perfuming of degraded product described in the step 5 concentration is 0.01-0.1%.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2006101600041A CN101209985A (en) | 2006-12-29 | 2006-12-29 | Method for extracting carotinoid from tobacco leaf by overcritical CO2 and application of the carotinoid in perfuming cigarette |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006101600041A CN101209985A (en) | 2006-12-29 | 2006-12-29 | Method for extracting carotinoid from tobacco leaf by overcritical CO2 and application of the carotinoid in perfuming cigarette |
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| CN101209985A true CN101209985A (en) | 2008-07-02 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102134527A (en) * | 2011-03-11 | 2011-07-27 | 郑州轻工业学院 | Method for preparing beta-carotene cigarette flavoring agent under ultrahigh pressure |
| CN101816949B (en) * | 2008-10-14 | 2011-09-14 | 中国林业科学研究院林产化学工业研究所 | Oxidization and degradation composite catalyst and use thereof in preparation of spice from carotenoid |
| CN102199490A (en) * | 2010-03-24 | 2011-09-28 | 郑州轻工业学院 | Method for extracting neutral aroma compositions in tobacco |
| CN102978004A (en) * | 2012-12-25 | 2013-03-20 | 华宝食用香精香料（上海）有限公司 | Preparation method and application of cigarette flavor |
| CN103087824A (en) * | 2013-01-31 | 2013-05-08 | 中国烟草总公司郑州烟草研究院 | Preparation method of cigarette flavor and application thereof |
| CN103525869A (en) * | 2013-10-18 | 2014-01-22 | 中国烟草总公司郑州烟草研究院 | Method for preparing cigarette flavour by xanthine oxidase (XO) degrading carotenoid and application of cigarette flavour |
| CN103783660A (en) * | 2014-01-22 | 2014-05-14 | 江苏中烟工业有限责任公司 | Supercritical extraction method of aroma substances in tobacco leaf fragments and application of aroma substances |
| CN104757704A (en) * | 2014-12-31 | 2015-07-08 | 贵州中烟工业有限责任公司 | Preparation method for tobacco extract and composition with the tobacco extract |
| RU2648452C1 (en) * | 2016-12-07 | 2018-03-26 | федеральное государственное бюджетное образовательное учреждение высшего образования "Волгоградский государственный медицинский университет" Министерства здравоохранения Российской Федерации | Method for obtaining individual carothynoids |
-
2006
- 2006-12-29 CN CNA2006101600041A patent/CN101209985A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101816949B (en) * | 2008-10-14 | 2011-09-14 | 中国林业科学研究院林产化学工业研究所 | Oxidization and degradation composite catalyst and use thereof in preparation of spice from carotenoid |
| CN102199490A (en) * | 2010-03-24 | 2011-09-28 | 郑州轻工业学院 | Method for extracting neutral aroma compositions in tobacco |
| CN102199490B (en) * | 2010-03-24 | 2012-11-21 | 郑州轻工业学院 | Method for extracting neutral aroma compositions in tobacco |
| CN102134527A (en) * | 2011-03-11 | 2011-07-27 | 郑州轻工业学院 | Method for preparing beta-carotene cigarette flavoring agent under ultrahigh pressure |
| CN102134527B (en) * | 2011-03-11 | 2013-05-01 | 郑州轻工业学院 | Method for preparing beta-carotene cigarette flavoring agent under ultrahigh pressure |
| CN102978004A (en) * | 2012-12-25 | 2013-03-20 | 华宝食用香精香料（上海）有限公司 | Preparation method and application of cigarette flavor |
| CN103087824A (en) * | 2013-01-31 | 2013-05-08 | 中国烟草总公司郑州烟草研究院 | Preparation method of cigarette flavor and application thereof |
| CN103087824B (en) * | 2013-01-31 | 2014-08-20 | 中国烟草总公司郑州烟草研究院 | Preparation method of cigarette flavor and application thereof |
| CN103525869A (en) * | 2013-10-18 | 2014-01-22 | 中国烟草总公司郑州烟草研究院 | Method for preparing cigarette flavour by xanthine oxidase (XO) degrading carotenoid and application of cigarette flavour |
| CN103525869B (en) * | 2013-10-18 | 2015-07-08 | 中国烟草总公司郑州烟草研究院 | Method for preparing cigarette flavour by xanthine oxidase (XO) degrading carotenoid and application of cigarette flavour |
| CN103783660A (en) * | 2014-01-22 | 2014-05-14 | 江苏中烟工业有限责任公司 | Supercritical extraction method of aroma substances in tobacco leaf fragments and application of aroma substances |
| CN103783660B (en) * | 2014-01-22 | 2015-11-18 | 江苏中烟工业有限责任公司 | The supercritical extraction method of flavor matter and application thereof in a kind of tobacco leaf fragment |
| CN104757704A (en) * | 2014-12-31 | 2015-07-08 | 贵州中烟工业有限责任公司 | Preparation method for tobacco extract and composition with the tobacco extract |
| CN104757704B (en) * | 2014-12-31 | 2019-06-07 | 贵州中烟工业有限责任公司 | A kind of preparation method of tobacco extract and composition containing the tobacco extract |
| RU2648452C1 (en) * | 2016-12-07 | 2018-03-26 | федеральное государственное бюджетное образовательное учреждение высшего образования "Волгоградский государственный медицинский университет" Министерства здравоохранения Российской Федерации | Method for obtaining individual carothynoids |
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Open date: 20080702 |