CN103183585A - Method for extracting solanesol by combining ultrasonic enzymic method and supercritical carbon dioxide - Google Patents
Method for extracting solanesol by combining ultrasonic enzymic method and supercritical carbon dioxide Download PDFInfo
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- CN103183585A CN103183585A CN201210527462XA CN201210527462A CN103183585A CN 103183585 A CN103183585 A CN 103183585A CN 201210527462X A CN201210527462X A CN 201210527462XA CN 201210527462 A CN201210527462 A CN 201210527462A CN 103183585 A CN103183585 A CN 103183585A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a method for extracting solanesol by combining an ultrasonic enzymic method and supercritical carbon dioxide. The method uses abandoned tobacco as the raw material, makes waste profitable, can promote economic development, has high economic benefits, combines a modern method, i.e. the ultrasonic enzymic method, and a supercritical carbon dioxide method, has high production efficiency and short time, reduces drainage of waste liquid, reduces environmental pollution and is a green and environmental-friendly production process.
Description
Technical field
The present invention relates to a kind of extracting method of eggplant Buddhist nun alcohol, particularly relating to a kind of is raw material with the inferior tobacco, and ultrasonic enzyme process extracts the method for eggplant Buddhist nun alcohol in conjunction with supercritical carbon dioxide extraction.
Background technology
Eggplant Buddhist nun alcohol (solanesol) is a kind of undersaturated isopolyprenols, belongs to long-chain hemiterpene alcohol and topples over thing, and molecular formula is C
45H
74O, relative molecular mass is 631, is a kind of white or pale yellow powder, is soluble in organic solvents such as normal hexane, acetone, sherwood oil, is insoluble in water.Eggplant Buddhist nun alcohol is a kind of important medicine intermediate, is mainly used in synthesizing coenzyme Q 10, vitamin K, anticancer synergist SDB etc.
Eggplant Buddhist nun alcohol extensively is present in the higher plant body with the form of free state and compound state, it is found that afterwards that eggplant Buddhist nun alcohol content was higher in the tobacco leaf, because China is the earth-shaking big country of tobacco, and the amount of abandoned tobacco can reach 1,500,000 tons, and therefore adopting inferior tobacco to extract eggplant Buddhist nun alcohol is an important application.The extracting method of eggplant Buddhist nun alcohol mainly contains organic solvent extraction method, dynamic saponifiable extraction method etc. in the prior art, but traditional extraction method exists production cost height, big, the problem of environment pollution caused of solvent consumption; Also there were some new extracting method to obtain development widely in recent years, and obtained certain effect.
Supercritical carbon dioxide extraction method is that a kind of supercritical co that utilizes has special solvency action to natural product, utilize the dissolving power of supercritical co and the relation of its density, namely utilize pressure and temperature that the influence of supercritical co dissolving power is carried out.Under supercritical state, supercritical co is contacted with material to be separated, extracting substance is then separated out fully or substantially, separates the purpose of purifying thereby reach.
Summary of the invention
The objective of the invention is to adopt a kind of new green non-pollution rapid technology from inferior tobacco, to extract eggplant Buddhist nun alcohol.
To be a kind of ultrasonic enzyme process extract the method for eggplant Buddhist nun alcohol in conjunction with supercritical carbon dioxide extraction in the present invention, comprises following step:
1) with after the dry inferior tobacco pulverizing, cross 10 ~ 30 mesh sieves and get Powdered offal, then crumbled tobacco and distilled water are pressed mass volume ratio 1g:20 ~ 40mL, be 200 ~ 250W at ultrasonic power, frequency is 40 ~ 60KHz, temperature is ultrasonic washing 40 ~ 60min under 50 ~ 55 ℃ of conditions, filter then solid matter A;
2) in substance A, add cellulase and the composite enzyme liquid of polygalacturonase, the mass volume ratio of crumbled tobacco and enzyme liquid is 1g:10 ~ 20mL, be 100 ~ 200W at ultrasonic power, ultrasound-assisted enzymolysis 30 ~ 45min under the condition of frequency 40KHZ, 45 ~ 50 ℃ of temperature, stirring velocity 30 ~ 50r/min, and under 4500 ~ 5000r/min condition centrifugal 15 ~ 20min, after the reject supernatant liquor substance B.
3) after substance B dissolves with 95% ethanol-normal hexane (2:1), be 200W at ultrasonic power, frequency is 40 KHZ, and temperature is ultrasonic 20min under 45 ~ 50 ℃ of conditions, and centrifugal 20min under 4000 ~ 4500r/min condition gets supernatant C then.
4) C is put in the extraction kettle, the sealing supercritical carbon dioxide extraction apparatus, extraction conditions is: adopt static extracting, carbon dioxide flow 20kg/h, pressure are 30 ~ 35MPa, and temperature is 39 ~ 45 ℃, and entrainment agent is 85 ~ 90% ethanol, and the dwell time is 3 ~ 6h; The release flow is 5kg/h, and reclaims venting end extract.With material in extract and the still merge purity at 85 ~ 90% eggplant Buddhist nun alcohol.
Wherein the addition of cellulase and polygalacturonase compositional liquor is: 300 ~ 500U/g:30 ~ 150U/g.
Compared with prior art, the invention has the beneficial effects as follows:
1) the present invention is raw material with the abandoned tobacco, turns waste into wealth, and can promote economic development the economic benefit height;
2) production efficiency height, the time is short, and has reduced discharging of waste liquid, has reduced environmental pollution, is a kind of green production process of environmental protection.
Embodiment
Embodiment 1:
Getting the offal of 10kg drying and screening, then crumbled tobacco and distilled water are pressed mass volume ratio 1g:20mL, is 200W at ultrasonic power, and frequency is 40KHz, and temperature is ultrasonic washing 40min under 50 ℃ of conditions, filter then solid matter A; In substance A, add 300U/g cellulase and the composite enzyme liquid of 30U/g polygalacturonase, the mass volume ratio of crumbled tobacco and enzyme liquid is 1g:10mL, be 100W at ultrasonic power, frequency 40KHZ, 45 ℃ of temperature, ultrasound-assisted enzymolysis 30min under the condition of stirring velocity 30r/min, and under the 4500r/min condition centrifugal 15min, get substance B after the reject supernatant liquor, with substance B with after 95% ethanol-normal hexane (2:1) dissolving, be 200W at ultrasonic power, frequency is 40 KHZ, temperature is ultrasonic 20min under 45 ℃ of conditions, and centrifugal 20min under the 4000r/min condition gets supernatant C then.C is put in the extraction kettle, the sealing supercritical carbon dioxide extraction apparatus, extraction conditions is: adopt static extracting, carbon dioxide flow 20kg/h, pressure are 30MPa, and temperature is 39 ℃, and entrainment agent is 90% ethanol, and the dwell time is 6h; The release flow is 5kg/h, and reclaims venting end extract.With material in extract and the still merge purity at 85% eggplant Buddhist nun alcohol 2.5kg.
Embodiment 2:
Getting the offal of 10kg drying and screening, then crumbled tobacco and distilled water are pressed mass volume ratio 1g:20mL, is 200W at ultrasonic power, and frequency is 40KHz, and temperature is ultrasonic washing 40min under 50 ℃ of conditions, filter then solid matter A; In substance A, add 500U/g cellulase and the composite enzyme liquid of 150U/g polygalacturonase, the mass volume ratio of crumbled tobacco and enzyme liquid is 1g:10mL, be 100W at ultrasonic power, frequency 40KHZ, 45 ℃ of temperature, ultrasound-assisted enzymolysis 30min under the condition of stirring velocity 30r/min, and under the 5000r/min condition centrifugal 15min, get substance B after the reject supernatant liquor, with substance B with after 95% ethanol-normal hexane (2:1) dissolving, be 200W at ultrasonic power, frequency is 40 KHZ, temperature is ultrasonic 20min under 50 ℃ of conditions, and centrifugal 20min under the 4000r/min condition gets supernatant C then.C is put in the extraction kettle, the sealing supercritical carbon dioxide extraction apparatus, extraction conditions is: adopt static extracting, carbon dioxide flow 20kg/h, pressure are 35MPa, and temperature is 45 ℃, and entrainment agent is 95% ethanol, and the dwell time is 3h; The release flow is 5kg/h, and reclaims venting end extract.With material in extract and the still merge purity at 90% eggplant Buddhist nun alcohol 2kg.
Claims (2)
1. a ultrasonic enzyme process extracts the method for eggplant Buddhist nun alcohol in conjunction with supercritical carbon dioxide extraction, it is characterized in that: comprise following step:
1) with after the dry inferior tobacco pulverizing, cross 10 ~ 30 mesh sieves and get Powdered offal, then crumbled tobacco and distilled water are pressed mass volume ratio 1g:20 ~ 40mL, be 200 ~ 250W at ultrasonic power, frequency is 40 ~ 60KHz, temperature is ultrasonic washing 40 ~ 60min under 50 ~ 55 ℃ of conditions, filter then solid matter A;
2) in substance A, add cellulase and the composite enzyme liquid of polygalacturonase, the mass volume ratio of crumbled tobacco and enzyme liquid is 1g:10 ~ 20mL, be 100 ~ 200W at ultrasonic power, ultrasound-assisted enzymolysis 30 ~ 45min under the condition of frequency 40KHZ, 45 ~ 50 ℃ of temperature, stirring velocity 30 ~ 50r/min, and under 4500 ~ 5000r/min condition centrifugal 15 ~ 20min, after the reject supernatant liquor substance B;
3) after substance B dissolves with 95% ethanol-normal hexane (2:1), be 200W at ultrasonic power, frequency is 40 KHz, and temperature is ultrasonic 20min under 45 ~ 50 ℃ of conditions, and centrifugal 20min under 4000 ~ 4500r/min condition gets supernatant C then;
4) C is put in the extraction kettle, the sealing supercritical carbon dioxide extraction apparatus, extraction conditions is: adopt static extracting, carbon dioxide flow 20kg/h, pressure are 30 ~ 35MPa, and temperature is 39 ~ 45 ℃, and entrainment agent is 85 ~ 90% ethanol, and the dwell time is 3 ~ 6h; The release flow is 5kg/h, and reclaims venting end extract;
With material in extract and the still merge purity at 85 ~ 90% eggplant Buddhist nun alcohol.
2. ultrasonic enzyme process as claimed in claim 1 is in conjunction with the method for supercritical carbon dioxide extraction extraction eggplant Buddhist nun alcohol, and it is characterized in that: the addition of cellulase and polygalacturonase compositional liquor is: 300 ~ 500U/g:30 ~ 150U/g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201210527462XA CN103183585A (en) | 2012-12-10 | 2012-12-10 | Method for extracting solanesol by combining ultrasonic enzymic method and supercritical carbon dioxide |
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| CN201210527462XA CN103183585A (en) | 2012-12-10 | 2012-12-10 | Method for extracting solanesol by combining ultrasonic enzymic method and supercritical carbon dioxide |
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| CN103183585A true CN103183585A (en) | 2013-07-03 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108285405A (en) * | 2018-01-10 | 2018-07-17 | 上海烟草集团有限责任公司 | A method of the rapid extraction Salanesol from industrial tobacco material waste |
| CN115039901A (en) * | 2022-05-19 | 2022-09-13 | 河北中烟工业有限责任公司 | Tobacco flavor, preparation method thereof and heated cigarette |
| CN115399498A (en) * | 2022-08-29 | 2022-11-29 | 河北中烟工业有限责任公司 | Tobacco extract, preparation method thereof and tobacco product |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1919816A (en) * | 2006-09-14 | 2007-02-28 | 浙江大学 | Preparation of high purity solanesol |
| CN101182284A (en) * | 2007-12-21 | 2008-05-21 | 中国科学院山西煤炭化学研究所 | Method for extracting high-purity solanesol from potato leaf, tobacco leaf and/or tobacco stem |
| CN101979613A (en) * | 2010-10-28 | 2011-02-23 | 西北师范大学 | Ultrasound enzyme-assisted solanesol extracting method |
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2012
- 2012-12-10 CN CN201210527462XA patent/CN103183585A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1919816A (en) * | 2006-09-14 | 2007-02-28 | 浙江大学 | Preparation of high purity solanesol |
| CN101182284A (en) * | 2007-12-21 | 2008-05-21 | 中国科学院山西煤炭化学研究所 | Method for extracting high-purity solanesol from potato leaf, tobacco leaf and/or tobacco stem |
| CN101979613A (en) * | 2010-10-28 | 2011-02-23 | 西北师范大学 | Ultrasound enzyme-assisted solanesol extracting method |
Non-Patent Citations (4)
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| 张歆等: "超临界CO2萃取烟草中茄尼醇", 《精细化工》 * |
| 王亚红等: "烟叶中茄尼醇提取精制与分析鉴定的研究进展", 《天津化工》 * |
| 赵良俊等: "混合溶剂与超声波辅助提取茄尼醇的工艺研究", 《精细化工中间体》 * |
| 逢敏洁: "烟草废弃物中茄尼醇等有效成分的提取分离与含量分析", 《中国优秀硕士学位论文全文数据库 农业科技辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108285405A (en) * | 2018-01-10 | 2018-07-17 | 上海烟草集团有限责任公司 | A method of the rapid extraction Salanesol from industrial tobacco material waste |
| CN115039901A (en) * | 2022-05-19 | 2022-09-13 | 河北中烟工业有限责任公司 | Tobacco flavor, preparation method thereof and heated cigarette |
| CN115399498A (en) * | 2022-08-29 | 2022-11-29 | 河北中烟工业有限责任公司 | Tobacco extract, preparation method thereof and tobacco product |
| CN115399498B (en) * | 2022-08-29 | 2023-06-27 | 河北中烟工业有限责任公司 | Tobacco extract, preparation method thereof and tobacco product |
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Application publication date: 20130703 |