CN1534008A - Method of extracting purified solanesol from tobacco leaf - Google Patents
Method of extracting purified solanesol from tobacco leaf Download PDFInfo
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- CN1534008A CN1534008A CNA2004100135611A CN200410013561A CN1534008A CN 1534008 A CN1534008 A CN 1534008A CN A2004100135611 A CNA2004100135611 A CN A2004100135611A CN 200410013561 A CN200410013561 A CN 200410013561A CN 1534008 A CN1534008 A CN 1534008A
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- tobacco leaf
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Abstract
A process for extracting high-purity solanesol from tobacco leaf includes mixing tobacco leaf with solvent, beating, filtering slurry, vacuum extracting of filtered cake in alcohol, filtering, collecting the filtrate, concentrating, saponfiying, extracting with n-hexane, washing with water, adsorbing, filtering, extracting the filtrate in alcohol, concentrating, freezing to educe out crystal, filtering, dissolving crystal in hot acetonitrile and low-temp educing of rystal twice. Its advantages are high purity (more than 95%), high output rate and low cost.
Description
Affiliated technical field
The present invention is a kind of method for purifying solanesol of extracting from tobacco leaf.
Background technology
At industrial eggplant Buddhist nun alcohol is synthesizing coenzyme Q
10And vitamin K
2Essential raw material.Ubiquinone
10Be the natural antioxidants that cell self produces, the activator of cellular metabolism can improve organic immunizing power.Studies show that in recent years, ubiquinone
10Aspect the treatment cardiovascular disorder unique curative effect is being arranged, aspect treatment vitamin C deficiency, duodenal ulcer and stomach ulcer, gangrenosum acne periodontitis, the viral hepatitis significant curative effect is being arranged, the experimentation on animals result shows ubiquinone
10Have antitumor action, being used to clinically cure changes acute cancer patients late period certain curative effect, ubiquinone is arranged
10Tablet is used for the treatment of circular baldness effectively, and pulmonary emphysema also have certain curative effect to the treatment of dysacousis, and find more that recently it has significant auxiliary curative effect to acquired immune deficiency syndrome (AIDS).Therefore as ubiquinone
10Extraction, the purifying of eggplant Buddhist nun alcohol that must synthesis material also more and more cause people's concern.The raw material that extracts eggplant Buddhist nun alcohol at present is dry tobacco leaf, extraction solvent mostly is industrial normal hexane or No. 6 organic solvents such as solvent, these class methods have following defective: one, do raw material with tobacco leaf, before extracting, need oven dry, with with new fresh tobacco leaf extract phase ratio, this has not only increased cost, and a part of eggplant Buddhist nun alcohol is degraded; Two, because the extraction solvent consumption is big, and boiling point is low, be difficult for reclaiming, cause solvent use cost height, there is the problem of fire safety evaluating hidden danger and air severe contamination simultaneously near and product cost height.
Summary of the invention
The objective of the invention is to overcome high energy consumption, low-yield, dirty environment in the present production technique and problem such as dye, seek a kind of operational path of new extraction purified solanesol.
The present invention is as a kind of method for purifying solanesol of extracting from tobacco leaf, its technical process is: tobacco leaf was mixed by mass ratio with 60～90% ethanol in 1: 2～1: 6, and pull an oar with hollander and to be Powdered to material, filter making beating liquid with 100～200 purpose filter clothes, filter cake changes cavitation suspendible liquid-solid extraction tripping device (patent No. is ZL 03211143.6) over to and carries out the cavitation extraction.Extraction liquid is concentrated into 1/10～1/15 of original volume with the merging of the filtrate of aforementioned making beating after filtration, concentrated solution adds the sodium hydroxide of 10-15% or the ethanolic soln of potassium hydroxide refluxed 30～60 minutes, carry out saponification reaction, react the after saponification liquid that finishes and change cavitation suspension liquid extracting and separating device (patent No. is ZL 03210970.9) over to, with n-hexane extraction with volume, n-hexane extract washes with water to neutrality, add gac or atlapulgite absorption 8～12 hours, adopt millipore filtration or the hollow fiber ultrafiltration membrane of 0.2～0.4 μ m to filter.Filtrate is used 80% alcohol extraction, concentrates the normal hexane phase and at-27～-35 ℃ of following freezing crystallizatioies, adopts 100～200 order filter clothes to filter crystal; Ratio in 70～110 liters of/kilogram dry materials is mixed above-mentioned crystal, dissolves, is placed crystallization in 12-16 hour down at 10～15 ℃ with the acetonitrile that is heated to 42～70 ℃, this process repeats once again, can obtain the eggplant Buddhist nun alcohol elaboration more than 95%.The present invention have eggplant Buddhist nun alcohol loss less, low, the eggplant Buddhist nun alcohol yield of technology cost and the high characteristics of purity.
The present invention is described further below by embodiment.
Embodiment one
Get 100 kilograms of fresh tobacco leafs, add 500 kilograms of 70% ethanol, the hollander making beating, filter making beating liquid, filter cake with the extraction of 80% ethanol cavitation, filters again, the filtrate of filtrate and aforementioned making beating merges concentrated, saponification, saponification liquor is with 10 liters of n-hexane extractions, and n-hexane extract washes with water to neutrality, adds 110 gram charcoal absorptions 10 hours.Tubular fibre filters, filtrate is with 80% alcohol extraction, normal hexane is concentrated into 1 liter ,-31 ℃ freezing crystallizatioies down mutually, filter crystal, crystal dissolves 15 ℃ of following crystallizatioies with 6 liters 60 ℃ acetonitrile, crystal is again with the dissolving of 4 liters 50 ℃ acetonitrile, 12 ℃ of following crystallizatioies obtain the eggplant Buddhist nun alcohol of purity 95.2%, yield 0.4%.
Embodiment two
Take from 100 kilograms on right exsiccant tobacco leaf, add 600 kilograms of 60% ethanol, the hollander making beating, filter making beating liquid, filter cake with the extraction of 70% ethanol cavitation, filters again, the filtrate of filtrate and aforementioned making beating merges concentrated, saponification, saponification liquor is with 20 liters of n-hexane extractions, and n-hexane extract washes with water to neutrality, adds 250 gram charcoal absorptions 8 hours.Filtering with microporous membrane, filtrate is with 80% alcohol extraction, normal hexane is concentrated into 2.5 liters ,-33 ℃ freezing crystallizatioies down mutually, filter crystal, crystal dissolves 13 ℃ of following crystallizatioies with 15 liters 50 ℃ acetonitrile, crystal is again with the dissolving of 12 liters 53 ℃ acetonitrile, 15 ℃ of following crystallizatioies obtain the eggplant Buddhist nun alcohol of purity 95.1%, yield 0.5%.
Embodiment three
Get 100 kilograms of fresh tobacco leafs, add 200 kilograms of 80% ethanol, the hollander making beating, filter making beating liquid, filter cake with the extraction of 80% ethanol cavitation, filters again, the filtrate of filtrate and aforementioned making beating merges concentrated, saponification, saponification liquor is with 15 liters of n-hexane extractions, and n-hexane extract washes with water to neutrality, adds 98 gram charcoal absorptions 12 hours.Filtering with microporous membrane, filtrate is with 70% alcohol extraction, normal hexane is concentrated into 1.1 liters ,-27 ℃ freezing crystallizatioies down mutually, filter crystal, crystal dissolves 13 ℃ of following crystallizatioies with 7 liters 52 ℃ acetonitrile, crystal is again with the dissolving of 5 liters 50 ℃ acetonitrile, 14 ℃ of following crystallizatioies obtain the eggplant Buddhist nun alcohol of purity 95.0%, yield 0.4%.
Claims (10)
1. one kind is extracted method for purifying solanesol from tobacco leaf, it is characterized in that tobacco leaf and solvent are mixed in proportion, and pull an oar with hollander, filter making beating liquid, filter cake is again with the extraction of ethanol cavitation, filter, the filtrate of filtrate and aforementioned making beating liquid merges concentrated, saponification, and saponification liquor n-hexane extraction, n-hexane extract wash with water to neutrality, add adsorbents adsorb certain hour after-filtration, filtrate is used alcohol extraction, concentrates normal hexane phase and freezing crystallization, filters crystal, crystal can obtain the eggplant Buddhist nun alcohol elaboration more than 95% with acetonitrile dissolving, the low temperature crystallization twice of heat.
2. by the described tobacco leaf of claim 1, it is characterized in that: can be the new fresh tobacco leaf of plucking, also can be the tobacco leaf through seasoning.
3. be mixed in proportion by described tobacco leaf of claim 1 and solvent, it is characterized in that, the solvent of making beating is 60～90% ethanol, and solvent and tobacco leaf blended mass ratio are 3: 1～6: 1.
4. by the described cavitation of claim 1, it is characterized in that with the negative pressure being that power carried out 30～60 minutes in cavitation suspendible liquid-solid extraction tripping device.
5. by the described extraction of claim 1, it is characterized in that with the negative pressure being that power extracted 5～10 minutes in cavitation suspension liquid extracting and separating device.
6. by the described absorption of claim 1, it is characterized in that sorbent material is gac or atlapulgite, adsorption time is 8～12 hours.
7. by the described filtration of claim 1, it is characterized in that adopting the millipore filtration of 0.2～0.4 μ m or hollow fiber ultrafiltration membrane to filter.
8. by the mutually freezing crystallization of the described normal hexane of claim 1, the temperature of crystallization is-27～-35 ℃.
9. it is characterized in that by the acetonitrile dissolving of the described crystal of claim 1 with heat: the temperature during acetonitrile dissolving crystal is 42～70 ℃; Acetonitrile and dissolved crystalline ratio are 70～110 liters of/kilogram dry materials.
10. it is characterized in that by the described low temperature crystallization of claim 1: the temperature during the low temperature crystallization is 10～15 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410013561 CN1250502C (en) | 2004-02-18 | 2004-02-18 | Method of extracting purified solanesol from tobacco leaf |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410013561 CN1250502C (en) | 2004-02-18 | 2004-02-18 | Method of extracting purified solanesol from tobacco leaf |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1534008A true CN1534008A (en) | 2004-10-06 |
| CN1250502C CN1250502C (en) | 2006-04-12 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410013561 Expired - Fee Related CN1250502C (en) | 2004-02-18 | 2004-02-18 | Method of extracting purified solanesol from tobacco leaf |
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| CN (1) | CN1250502C (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100396654C (en) * | 2005-12-07 | 2008-06-25 | 兰州众翼化工有限公司 | Method for extracting high-purity solanesol from potato leaf |
| CN100398100C (en) * | 2005-09-27 | 2008-07-02 | 四川大学 | Method for extracting high-content solanesol extract by liquid-liquid two-phase method |
| CN100410222C (en) * | 2006-02-13 | 2008-08-13 | 李祥庆 | Method for extracting high purity solanesol from low content solanesol extract |
| US7649120B2 (en) | 2008-02-20 | 2010-01-19 | Northwest Normal University | Microwave-assisted extraction of solanesol from potato stems and/or leaves |
| CN102408312A (en) * | 2011-11-30 | 2012-04-11 | 薛刚 | Method for separating and purifying solanesol through subsection crystallization |
| CN105124740A (en) * | 2015-08-28 | 2015-12-09 | 湖北中烟工业有限责任公司 | Method for freezing and concentrating paper-making reconstituted tobacco refined liquid |
| CN105646150A (en) * | 2016-02-03 | 2016-06-08 | 河西学院 | Method for extracting high-purity solanesol from tobacco leaves |
-
2004
- 2004-02-18 CN CN 200410013561 patent/CN1250502C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100398100C (en) * | 2005-09-27 | 2008-07-02 | 四川大学 | Method for extracting high-content solanesol extract by liquid-liquid two-phase method |
| CN100396654C (en) * | 2005-12-07 | 2008-06-25 | 兰州众翼化工有限公司 | Method for extracting high-purity solanesol from potato leaf |
| CN100410222C (en) * | 2006-02-13 | 2008-08-13 | 李祥庆 | Method for extracting high purity solanesol from low content solanesol extract |
| US7649120B2 (en) | 2008-02-20 | 2010-01-19 | Northwest Normal University | Microwave-assisted extraction of solanesol from potato stems and/or leaves |
| CN102408312A (en) * | 2011-11-30 | 2012-04-11 | 薛刚 | Method for separating and purifying solanesol through subsection crystallization |
| CN102408312B (en) * | 2011-11-30 | 2014-04-09 | 南阳理工学院 | Method for separating and purifying solanesol through subsection crystallization |
| CN105124740A (en) * | 2015-08-28 | 2015-12-09 | 湖北中烟工业有限责任公司 | Method for freezing and concentrating paper-making reconstituted tobacco refined liquid |
| CN105646150A (en) * | 2016-02-03 | 2016-06-08 | 河西学院 | Method for extracting high-purity solanesol from tobacco leaves |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1250502C (en) | 2006-04-12 |
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