CN1250502C - Method of extracting purified solanesol from tobacco leaf - Google Patents
Method of extracting purified solanesol from tobacco leaf Download PDFInfo
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- CN1250502C CN1250502C CN 200410013561 CN200410013561A CN1250502C CN 1250502 C CN1250502 C CN 1250502C CN 200410013561 CN200410013561 CN 200410013561 CN 200410013561 A CN200410013561 A CN 200410013561A CN 1250502 C CN1250502 C CN 1250502C
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- tobacco leaf
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Abstract
The present invention relates to a method for extracting and purifying solanesol from tobacco, whose process flow comprises: tobacco and a solvent are proportionally mixed and are pulped by a pulping machine, pulp is filtered, and a filter cake is extracted by cavitation by ethanol and is filtered. A filtered solution and the filtered solution of the pulp are combined, concentrated and saponified, and a saponified solution is extracted by n-hexane. An n-hexane extract is washed by water to be neutral and is filtered after an absorbing agent is added to carry out absorption for certain time, and a filtered solution is extracted by the ethanol. An n-hexane phase is concentrated and is crystallized by freezing, crystals are filtered and are dissolved by hot acetonitrile, low temperature crystallization is carried out twice, and fine solanesol products whose purity is more than 95% can be obtained. The present invention has the characteristics of little loss of the solanesol, low technological cost, and high yield and high purity of the solanesol.
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 problems such as high energy consumption in the present production technique, low-yield, environmental pollution, 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, with the negative pressure is power, in cavitation suspendible liquid-solid extraction tripping device (patent No. is ZL 03211143.6) the filter cake cavitation is extracted 30-60 minute.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 the negative pressure is power, with n-hexane extraction 5-10 minute 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 (8)
1. one kind is extracted method for purifying solanesol from tobacco leaf, comprises the steps:
(1) making beating
Tobacco leaf and solvent are mixed in proportion, and with the hollander making beating, filter making beating liquid, get filtrate and filter cake;
(2) negative pressure cavitation liquid-solid extraction
With the negative pressure is that power is used alcohol extraction 30～60 minutes to the described filter cake of step 1 in cavitation suspendible liquid-solid extraction tripping device, filters extraction liquid, and the merging of the filtrate of the described making beating liquid of filtrate and step 1 concentrates, and gets concentrated solution;
(3) saponification
The sodium hydroxide of the described concentrated solution adding of step 2 10-15% or the ethanolic soln of potassium hydroxide were refluxed 30～60 minutes, carry out saponification reaction, get saponification liquor;
(4) negative pressure cavitation liquid-liquid extraction
With the negative pressure is power, the described saponification liquor of step 3 was extracted 5～10 minutes in cavitation suspension liquid extracting and separating device with normal hexane, n-hexane extract washes with water to neutrality and adds adsorbents adsorb certain hour after-filtration, and filtrate is used alcohol extraction, normal hexane mutually with ethanol two portions mutually;
(5) crystallization
The described normal hexanes of enrichment step 4 mutually and freezing crystallizatioies filter crystal, and crystal obtains the pure elaboration of eggplant Buddhist nun 95% or more with acetonitrile dissolving, the low temperature crystallization twice of heat.
2. in accordance with the method for claim 1, wherein the described tobacco leaf of step 1 can be the new fresh tobacco leaf of plucking, and also can be the tobacco leaf through seasoning.
3. in accordance with the method for claim 1, wherein described tobacco leaf of step 1 and solvent are mixed in proportion, and it is characterized in that, the solvent of making beating is 60～90% ethanol, and the mass ratio of tobacco leaf and solvent is 1: 2～1: 6.
4. in accordance with the method for claim 1, the wherein absorption of the described n-hexane extract of step 4 is characterized in that sorbent material is gac or atlapulgite, and adsorption time is 8～12 hours.
5. in accordance with the method for claim 1, the wherein described filtration of step 4 is characterized in that adopting the millipore filtration of 0.2～0.4 μ m or hollow fiber ultrafiltration membrane to filter.
6. in accordance with the method for claim 1, the mutually freezing crystallization of the described normal hexane of step 5 wherein, the temperature of crystallization is-27～-35 ℃.
7. in accordance with the method for claim 1, wherein the described crystal of step 5 is characterized in that with hot acetonitrile dissolving: the temperature during acetonitrile dissolving crystal is 42～70 ℃; Acetonitrile and dissolved crystalline ratio are 70～110 liters of/kilogram dry materials.
8. in accordance with the method for claim 1, wherein the described low temperature crystallization of step 5 is characterized in that: 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 |
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| CN1534008A CN1534008A (en) | 2004-10-06 |
| CN1250502C true CN1250502C (en) | 2006-04-12 |
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| Application Number | Title | Priority Date | Filing Date |
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| 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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Families Citing this family (7)
| 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 |
| CN101284765B (en) | 2008-02-20 | 2011-03-30 | 西北师范大学 | Process for abstracting solanesol in waste of white potato haulm auxiliary by microwave |
| CN102408312B (en) * | 2011-11-30 | 2014-04-09 | 南阳理工学院 | Method for separating and purifying solanesol through subsection crystallization |
| CN105124740B (en) * | 2015-08-28 | 2017-02-01 | 湖北中烟工业有限责任公司 | Method for freezing and concentrating paper-making reconstituted tobacco refined liquid |
| CN105646150B (en) * | 2016-02-03 | 2018-08-17 | 河西学院 | A method of the extraction of high purity solanesol alcohol from tobacco leaf |
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2004
- 2004-02-18 CN CN 200410013561 patent/CN1250502C/en not_active Expired - Fee Related
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| CN1534008A (en) | 2004-10-06 |
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