CN1821196A - Method for extracting high purity solanesol from low content solanesol extract - Google Patents
Method for extracting high purity solanesol from low content solanesol extract Download PDFInfo
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- CN1821196A CN1821196A CN 200610038249 CN200610038249A CN1821196A CN 1821196 A CN1821196 A CN 1821196A CN 200610038249 CN200610038249 CN 200610038249 CN 200610038249 A CN200610038249 A CN 200610038249A CN 1821196 A CN1821196 A CN 1821196A
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Abstract
The process of extracting high purity solanesol from low content solanesol extractum of purity over 8 % includes the following steps: dissolving the extractum in the solvent I, saponification, extracting the saponified liquid with target solvent II, laminating, concentration, dissolving the concentrate with solvent III, crystallizing in a continuous crystallization system, centrifugal filtering, collecting the filter cake, decompressing to eliminate solvent, secondary crystallization with the solvent IV, and drying to obtain purified solanesol product. The process can reach solanesol product purity over 95 % and total solanesol yield over 85 %. The process uses no mixed solvent and is favorable to recovery of solvent.
Description
Technical field:
The present invention relates to a kind of from the method for content greater than extraction high-purity solanesol 8% the solanesol extract.Belong to technical field of chemistry.
Background technology:
The English name of eggplant Buddhist nun alcohol is Solanesol, and chemical name is 3,7,11,15,19,23,27,31,35-nine methyl-2,6,10,14,18,22,26,30, and 34-hexatriacontane nine rare-1-alcohol, molecular formula is H[CH
2C (CH
2) CHCH2] 9OH, molecular weight is 631.Pure product are white mealy crystal, 41 ℃ of fusing points.It is synthesizing coenzyme Q
10And vitamin K
2Essential raw material.And ubiquinone
10Be the natural antioxidants that cell self produces, the activator of cellular metabolism can improve organic immunizing power.Studies show that ubiquinone
10Aspect the treatment cardiovascular and cerebrovascular diseases unique curative effect is being arranged, in treatment leukemia, duodenal ulcer and stomach ulcer, the gangrenosum acne periodontitis, there is significant curative effect the viral hepatitis aspect.In recent years, ubiquinone
10Antitumor action also be it is found that.Therefore as ubiquinone
10The extraction and purification process of the eggplant Buddhist nun alcohol of synthesis material is more and more paid close attention to by people, particularly highly purified eggplant Buddhist nun alcohol product.
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 solvent wet goods organic solvents, and extract the method for elaboration eggplant Buddhist nun alcohol or adopt the eggplant Buddhist nun alcohol product of content＞70% is raw material, the raw materials cost height, source of supply limited (the domestic eggplant Buddhist nun alcohol that minority manufacturer production 70% content is only arranged at present).Or adopt silica gel chromatographic column to separate, and it is long to have the time, and purge process needs to pressurize shortcomings such as cost height.
The objective of the invention is to overcome above-mentioned deficiency, a kind of eggplant Buddhist nun alcohol yield and purity height are provided, equipment is simple, the method for extracting high-purity solanesol from the low levels solanesol extract that the technology cost is low.
The object of the present invention is achieved like this: a kind of method of extracting high-purity solanesol from the low levels solanesol extract, it is to adopt purity to make raw material greater than 8% solanesol extract, with solvent I dissolving after saponification, saponification liquor is through having the extraction of target solvent II, layering, concentrate, product after concentrating is passed through the crystallization of continuous crystallisation system with solvent II I dissolving back, centrifuging, collect filter cake, removal of solvent under reduced pressure re-uses solvent IV and carries out secondary crystal, centrifuging, drying gets the high-purity solanesol finished product.
The present invention extracts the method for high-purity solanesol from the low levels solanesol extract, its processing step is as follows:
Step 1, saponification are solanesol extract 8% or more with solvent I dissolving content, and solanesol extract: solvent I is 1: 2～5V/V, is heated to 35～70 ℃, adds alkali lye stirring 2～6h,
Step 2, extraction add solvent II, and the dosage of solvent II is 0.4～0.6 times, and 35 ℃～55 ℃ are stirred 15min～30min, and standing demix 1～1.5h abandons lower floor's water,
Step 3, concentrate step 2 got the organic phase concentrating under reduced pressure, be concentrated into solvent under the 0.01MPa negative pressure and no longer steam,
Step 4, crystallization get concentrated solution with 10 times～20 times solvent II I dissolving with step 3, filter, filtrate under-40 ℃～10 ℃ conditions in continuous crystallisation equipment crystallization separate out eggplant Buddhist nun alcohol, filter, obtain eggplant Buddhist nun alcohol filter cake, mother liquor reclaims,
Step 5, secondary crystal solvent-applied IV carry out secondary crystal with step 4, and Tc is-40 ℃～10 ℃, filter, and get eggplant Buddhist nun alcohol filter cake;
Step 6, drying get eggplant Buddhist nun alcohol filter cake with step 5 and be drying to obtain highly purified eggplant Buddhist nun alcohol finished product under 15～35 ℃ of temperature, condition of normal pressure.
The present invention extracts the method for high-purity solanesol from the low levels solanesol extract, the described solanesol extract raw material of step 1 greater than 8% be by extract in tobacco leaf, leaf of potato or the animal viscera, concentrate, products therefrom after the crystallization.Here 8% indication is the minimum content of this processing requirement solanesol extract, and solanesol extract content is 15～17% usually.
The present invention extracts the method for high-purity solanesol from the low levels solanesol extract,
The described solvent I of step 1 be Virahol ethyl acetate the trimethyl carbinol acetone chloroform tetracol phenixin methyl chloride, 1, the 2-ethylene dichloride hexanaphthene whiteruss dithiocarbonic anhydride benzene, toluene ether,
The described solvent II of step 2 be different from the described solvent I of step 1 Virahol ethyl acetate the trimethyl carbinol acetone chloroform tetracol phenixin methyl chloride, 1, the 2-ethylene dichloride hexanaphthene whiteruss dithiocarbonic anhydride benzene, toluene ether
The described solvent II I of step 4 be Virahol acetonitrile propyl carbinol the trimethyl carbinol acetone DMF ethyl acetate Glacial acetic acid glycerine,
The described solvent IV of step 5 be different from the described solvent II I of step 4 Virahol propyl carbinol the trimethyl carbinol acetone DMF ethyl acetate Glacial acetic acid glycerine.
The present invention extracts the method for high-purity solanesol from the low levels solanesol extract, it is characterized in that step 4, five described continuous crystallisation equipment are made of crystallizer and well heater, condenser parts.
The present invention has overcome problems such as high energy consumption in the present production technique, low-yield, contaminate environment, sought a kind of new be fit to and to can be applicable to industrialized facility investment little, technology is simple, do not need the chromatography process, there is not extreme condition, in the normal pressure less energy-consumption of work down, low cost, the operational path of the high-purity solanesol of constant product quality.Finally, can reach content and surpass 95% high-purity solanesol, eggplant Buddhist nun alcohol total recovery＞85%.Therefore the present invention has eggplant Buddhist nun alcohol yield and purity height, and equipment is simple, the characteristics that the technology cost is extremely low.Another benefit of the present invention is exactly not use mixed solvent, for solvent recovery afterwards brings great convenience.
Description of drawings:
Fig. 1 is technological process of production figure of the present invention.
Embodiment:
Embodiment 1: getting content is 8% solanesol extract 100g, adds toluene 300ml dissolving, adds alkali lye 15ml, and 70 ℃ are stirred 4h.Then, add Virahol 50ml, 50 ℃ are stirred 30min, leave standstill and abandon lower floor's water.Organic phase is evaporated to solvent no longer to steam.With 20 times acetone solution, filter.Filtrate under-40 ℃～-10 ℃ conditions in continuous crystallisation equipment crystallization separate out eggplant Buddhist nun alcohol, filter, resultant eggplant Buddhist nun alcohol filter cake carries out secondary crystal with Virahol again.Dry cake obtains the eggplant Buddhist nun alcohol of purity 95.7%, yield 85.8%.
Embodiment 2:
Getting content is 9% solanesol extract 300Kg, adds ethyl acetate 1000L dissolving, adds alkali lye 70L again, and 60 ℃ are stirred 5h.Then, add ethyl acetate 180L, 50 ℃ of stirring 30min leave standstill and abandon lower floor's water.Be evaporated to dried in 80 ℃ organic phase.With the acetone solution of 3000L, to filter, filtrate is separated out eggplant Buddhist nun alcohol under-40 ℃～-10 ℃ conditions, filter, and resultant eggplant Buddhist nun alcohol filter cake carries out secondary crystal with Virahol again.Drying obtains the eggplant Buddhist nun alcohol of purity 95.2%, yield 86.1%.
Claims (5)
1, a kind of method of from the low levels solanesol extract, extracting high-purity solanesol, it is characterized in that it is to adopt purity to make raw material greater than 8% solanesol extract, with solvent I dissolving after saponification, saponification liquor is through having the extraction of target solvent II, layering, concentrate, product after concentrating is passed through the crystallization of continuous crystallisation system with solvent II I dissolving back, and filter cake is collected in centrifuging, removal of solvent under reduced pressure, re-use solvent IV and carry out secondary crystal, drying gets the high-purity solanesol finished product.
2, a kind of method of from the low levels solanesol extract, extracting high-purity solanesol according to claim 1, it is characterized in that: its processing step is as follows:
Step 1, saponification are solanesol extract 8% or more with solvent I dissolving content, and solanesol extract: solvent I is 1: 2～5V/V, is heated to 35～70 ℃, adds alkali lye stirring 2～6h,
Step 2, extraction add solvent II, and the dosage of solvent II is 0.4～0.6 times, and 35 ℃～55 ℃ are stirred 15min～30min, and standing demix 1～1.5h abandons lower floor's water,
Step 3, concentrate step 2 got the organic phase concentrating under reduced pressure, be concentrated into solvent under the 0.01MPa negative pressure and no longer steam,
Step 4, crystallization get concentrated solution with 10 times～20 times solvent II I dissolving with step 3, filter, filtrate under-40 ℃～10 ℃ conditions in continuous crystallisation equipment crystallization separate out eggplant Buddhist nun alcohol, filter, obtain eggplant Buddhist nun alcohol filter cake, mother liquor reclaims,
Step 5, secondary crystal solvent-applied IV carry out secondary crystal with step 4, and Tc is-40 ℃～10 ℃, filter, and get eggplant Buddhist nun alcohol filter cake;
Step 6, drying get eggplant Buddhist nun alcohol filter cake with step 5 and be drying to obtain highly purified eggplant Buddhist nun alcohol finished product under 15～35 ℃ of temperature, condition of normal pressure.
3, a kind of method of extracting high-purity solanesol from the low levels solanesol extract according to claim 2 is characterized in that:
The described solanesol extract raw material of step 1 greater than 8% be by extract in tobacco leaf, leaf of potato or the animal viscera, concentrate, products therefrom after the crystallization.
4, a kind of method of extracting high-purity solanesol from the low levels solanesol extract according to claim 2 is characterized in that:
The described solvent I of step 1 be Virahol ethyl acetate the trimethyl carbinol acetone chloroform tetracol phenixin methyl chloride, 1, the 2-ethylene dichloride hexanaphthene whiteruss dithiocarbonic anhydride benzene, toluene ether,
The described solvent II of step 2 be different from the described solvent I of step 1 Virahol ethyl acetate the trimethyl carbinol acetone chloroform tetracol phenixin methyl chloride, 1, the 2-ethylene dichloride hexanaphthene whiteruss dithiocarbonic anhydride benzene, toluene ether
The described solvent II I of step 4 be Virahol acetonitrile propyl carbinol the trimethyl carbinol acetone DMF ethyl acetate Glacial acetic acid glycerine,
The described solvent IV of step 5 be different from the described solvent II I of step 4 Virahol propyl carbinol the trimethyl carbinol acetone DMF ethyl acetate Glacial acetic acid glycerine.
5, a kind of method of extracting high-purity solanesol from the low levels solanesol extract according to claim 2 is characterized in that step 4, five described continuous crystallisation equipment are made of crystallizer and well heater, condenser parts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100382497A CN100410222C (en) | 2006-02-13 | 2006-02-13 | Method for extracting high purity solanesol from low content solanesol extract |
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|---|---|---|---|
| CNB2006100382497A CN100410222C (en) | 2006-02-13 | 2006-02-13 | Method for extracting high purity solanesol from low content solanesol extract |
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| CN1821196A true CN1821196A (en) | 2006-08-23 |
| CN100410222C CN100410222C (en) | 2008-08-13 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100548954C (en) * | 2007-12-21 | 2009-10-14 | 中国科学院山西煤炭化学研究所 | From leaf of potato, tobacco leaf and/or tobacco rod, extract the method for high-purity solanesol |
| CN101284766B (en) * | 2008-06-04 | 2010-04-21 | 云南瑞升烟草技术（集团）有限公司 | Process for finely purifying high-purity solanesol form coarse cream of solanesol |
| CN102408311A (en) * | 2011-11-30 | 2012-04-11 | 薛刚 | Method for purifying solanesol through urea adduction fractionation |
| CN102408312A (en) * | 2011-11-30 | 2012-04-11 | 薛刚 | Method for separating and purifying solanesol through subsection crystallization |
| CN102816050A (en) * | 2012-09-13 | 2012-12-12 | 王星敏 | Method for extracting solanesol by activating waste and defective tobacco by enzyme catalysis |
| CN110143879A (en) * | 2019-04-29 | 2019-08-20 | 南京师范大学 | A kind of by-product that p-nitroacetophenone preparation generates carries out the device and method of recycling |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54138510A (en) * | 1978-04-19 | 1979-10-27 | Wakamoto Pharma Co Ltd | Method of gathering solanesol |
| JPS56104820A (en) * | 1980-01-25 | 1981-08-20 | Ajinomoto Co Inc | Preparation of unsaponified tobacco extract |
| CN1250502C (en) * | 2004-02-18 | 2006-04-12 | 东北林业大学 | Method of extracting purified solanesol from tobacco leaf |
-
2006
- 2006-02-13 CN CNB2006100382497A patent/CN100410222C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100548954C (en) * | 2007-12-21 | 2009-10-14 | 中国科学院山西煤炭化学研究所 | From leaf of potato, tobacco leaf and/or tobacco rod, extract the method for high-purity solanesol |
| CN101284766B (en) * | 2008-06-04 | 2010-04-21 | 云南瑞升烟草技术（集团）有限公司 | Process for finely purifying high-purity solanesol form coarse cream of solanesol |
| CN102408311A (en) * | 2011-11-30 | 2012-04-11 | 薛刚 | Method for purifying solanesol through urea adduction fractionation |
| 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 |
| CN102408311B (en) * | 2011-11-30 | 2014-04-09 | 南阳理工学院 | Method for purifying solanesol through urea adduction fractionation |
| CN102816050A (en) * | 2012-09-13 | 2012-12-12 | 王星敏 | Method for extracting solanesol by activating waste and defective tobacco by enzyme catalysis |
| CN110143879A (en) * | 2019-04-29 | 2019-08-20 | 南京师范大学 | A kind of by-product that p-nitroacetophenone preparation generates carries out the device and method of recycling |
| CN110143879B (en) * | 2019-04-29 | 2022-07-12 | 南京师范大学 | Device and method for recycling by-products generated in preparation of p-nitroacetophenone |
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| Publication number | Publication date |
|---|---|
| CN100410222C (en) | 2008-08-13 |
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Assignee: JIANGYIN XIANGYANG TECHNOLOGY CO., LTD. Assignor: Li Xiangqing Contract fulfillment period: 2009.4.10 to 2014.4.10 Contract record no.: 2009320000678 Denomination of invention: Method for extracting high purity solanesol from low content solanesol extract Granted publication date: 20080813 License type: Exclusive license Record date: 20090423 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.4.10 TO 2014.4.10; CHANGE OF CONTRACT Name of requester: JIANGYIN CITY XIANGYANG SCIENCE CO., LTD. Effective date: 20090423 |
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Granted publication date: 20080813 Termination date: 20200213 |