CN104072336A - Process for extracting solanesol - Google Patents
Process for extracting solanesol Download PDFInfo
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- CN104072336A CN104072336A CN201410250187.0A CN201410250187A CN104072336A CN 104072336 A CN104072336 A CN 104072336A CN 201410250187 A CN201410250187 A CN 201410250187A CN 104072336 A CN104072336 A CN 104072336A
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- extraction
- salanesol
- technique
- extraction kettle
- sorbent material
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a process for extracting solanesol. In the process, an important drug intermediate is directly extracted and separated from waste tobacco leaves by adopting a supercritical chromatography method. The process comprises the following steps: preprocessing raw materials, performing first-stage extraction, second-stage extraction and third-stage extraction in sequence, eluting, re-crystallizing, filtering and drying. According to the process, extraction and purification are combined together, a product with relatively high purity is obtained in one step, the process is different from a conventional two-step production process route of performing supercritical extraction at first and then performing chromatographic column purification, the process is simple, the extraction rate is high, the product purity is high, and the process has the advantages of no environmental pollution and the like.
Description
Technical field
The present invention relates to a kind of technique of extracting Salanesol.
Background technology
Salanesol is the synthetic important source material of medicine, is the irreplaceable key intermediate of ubiquinone class medicine, i.e. the side chain key of Coenzyme Q10 99.0 and multiprenylmenaquinone.Be widely used in the treatment of cardiovascular system diseases, also there is the body immunity of raising simultaneously, strengthen effect anti-oxidant, that retain youth, thereby widely apply at medicine, healthcare products and cosmetic field.
The method of current domestic extraction Salanesol mainly adopts the extracting method such as organic solvent extraction, molecular distillation method, thiocarbamide inclusion method and polymeric form co-precipitation, in these methods, exist operation steps many, solvent-oil ratio is large, effective component extraction rate is not high, cannot obtain highly purified product, and have comparatively serious problem of environmental pollution.Domestic the having been reported of technological method of overcritical purifying solanesol, as the patent of publication number CN1676502, is that to take the low levels Salanesol that organic solvent extraction method obtains be to extract raw material, adopts supercritical CO
2the production technique of processing, obtains purity and is 95% product.This invention, for the further refining processing of the Salanesol of low levels, cannot fundamentally solve the problem of environmental pollution that organic solvent extraction causes.The patent of publication number CN1817834A, key step comprises: through pretreated tobacco leaf picking entrainment agent intensifying technology, through supercritical CO
2the extraction of fluid one-level by the second-order separation, makes supercritical CO simultaneously
2the extract of fluid is optionally separated out in two different extraction kettles, has realized the first separated of Salanesol enrichment and extract, and it is more than 95% Salanesol that the further purifying of process column chromatography obtains purity.This patent adopts organic solvent as entrainment agent, causes on the one hand environmental pollution, can consume mass energy on the other hand when removing solvent; Supercritical CO
2the elementary Salanesol extracting is further purified and is obtained more than 95% Salanesol through saponification with through chromatography column, uses NaOH and sherwood oil during saponification, also can cause environmental pollution.This invention is through supercritical CO
2the methods such as the further purification of primary extraction, saponification and column chromatography, process is comparatively complicated.
Summary of the invention
Of the present invention for above-mentioned deficiency of the prior art, provide a kind of technique of extracting Salanesol, the advantage such as it is simple that the method has technique, and extraction yield is high, and product purity is high, non-environmental-pollution.
For achieving the above object, the present invention is achieved through the following technical solutions:
A technique of extracting Salanesol, comprises the following steps: recrystallization, filtration and be dried after the extraction of raw materials pretreatment, one-level, secondary extraction, three grades of extractions, wash-out.
A technique of extracting Salanesol, specifically comprises the following steps:
1) raw materials pretreatment: by drying tobacco and pulverizing; Preferably tobacco leaf is removed and gone mouldy tobacco leaf and impurity and reject offal, then dry and pulverizing;
2) one-level extraction: add the first extraction kettle to carry out the first of Salanesol pretreated raw material and carry, the first extraction kettle raw material filling ratio is 80%, and extracting pressure is 28-32Mpa, and temperature is 65-75 ℃, CO
2flow is 10L/h;
3) secondary extraction: the second extraction kettle that the effluent of the first extraction kettle directly enters with the first sorbent material dewaxes, degreasing and impurity elimination, the second extraction kettle pressure is 26-28Mpa, temperature is 60-70 ℃;
4) three grades of extractions: the effluent of the second extraction kettle enters in the 3rd extraction kettle with the second sorbent material, and this kind of sorbent material can optionally absorb Salanesol, and the 3rd extraction kettle pressure is 23-25Mpa, and temperature is 45-60 ℃;
5) recrystallization after wash-out: carry out wash-out, recrystallization after extraction finishes;
6) after filtration and dry recrystallization thing, obtain high purity (purity is more than 95%) Salanesol.
The effluent of above-mentioned the 3rd extraction kettle obtains by product through separating still, and described byproduct is tobacco flavor matter, comprises essential oil of tobaccos.
Described the first sorbent material is molecular sieve (preferably 10X molecular sieve or 5A molecular sieve), aluminium sesquioxide or gac.
Described the second sorbent material is chromatography silica gel (preferably 200-300 order) or resin (preferably AB-8).
Described wash-out is the mixture by sherwood oil and ethyl acetate, and volume ratio is 3.5:0.5-1.5 (preferably 4:1).
Described recrystallization is for carrying out with sherwood oil under-10--25 ℃ of (preferably-18 ℃) condition.
Described step 1) be preferably dried to water content and be less than 2%, grinding particle size is 20-40 order.
Beneficial effect of the present invention:
Overcritical chromatography is a kind of a kind of extraction process that supercritical extraction and chromatography are combined, extracting with purification, combine, one step obtains the product of higher degree, be different from traditional supercritical extraction of first using, the two step production process routes of then purifying with chromatography column, it utilizes supercritical CO
2good selectivity and the selection absorption of resin extract separated and purifying.
The method technique is simple, and extraction yield is high, and product purity is high, does not need the advantages such as entrainment agent, non-environmental-pollution.
Whole leaching process carries out successively, is continuous process, and whole extraction time is 75-90min.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
1) raw materials pretreatment: inferior tobacco is removed and to be gone mouldy tobacco leaf and impurity and to reject offal, be then dried to water content and be less than 2% and to be crushed to granularity be 20-40 order;
2) one-level extraction: add the first extraction kettle to carry out the first of Salanesol pretreated raw material and carry, wherein the first extraction kettle raw material filling ratio is 80%, and extracting pressure is 28Mpa, and temperature is 75 ℃, CO
2flow is 10L/h, and the whole components dissolved that can dissolve in tobacco leaf in the first extraction kettle are at supercritical CO
2in fluid, obtain comprising the fluid mixture of Salanesol;
3) secondary extraction: the second extraction kettle that the effluent of the first extraction kettle directly enters with 10X adsorbent of molecular sieve dewaxes, and degreasing and impurity elimination are rich in supercritical CO Salanesol
2in fluid, the second extraction kettle pressure is 26Mpa, and temperature is 70 ℃;
4) three grades of extractions: the effluent of the second extraction kettle enters in the 3rd extraction kettle with 200 object chromatography silica gel sorbent materials, this kind of sorbent material can optionally absorb Salanesol, the third extraction kettle pressure is 23Mpa, temperature is 60 ℃, the tobacco flavor matter that comprises tobacco cleaned oil flowing out from the 3rd extraction kettle carries out separation in separating still, obtain the by product of this invention, for the blending of high-grade cigarette;
5) fractionation by adsorption and recrystallization: it is sherwood oil by volume ratio that extraction finishes rear: the eluent that ethyl acetate is 4:1 carries out wash-out the 3rd extraction kettle, under-18 ℃ of conditions, with sherwood oil, carry out recrystallization afterwards, filter, be dried after recrystallization thing, obtain white flour, through HPLC, detect, the Salanesol purity of extraction is 95.8%.
Embodiment 2
1) raw materials pretreatment: inferior tobacco is removed and to be gone mouldy tobacco leaf and impurity and to reject offal, be then dried to water content and be less than 2% and to be crushed to granularity be 20-40 order;
2) one-level extraction: add the first extraction kettle to carry out the first of Salanesol pretreated raw material and carry, wherein the first extraction kettle raw material filling ratio is 80%, and extracting pressure is 32Mpa, and temperature is 65 ℃, CO
2flow is 10L/h, and the whole components dissolved that can dissolve in tobacco leaf in the first extraction kettle are at supercritical CO
2in fluid, obtain comprising the fluid mixture of Salanesol;
3) secondary extraction: the second extraction kettle that the effluent of the first extraction kettle directly enters with aluminium sesquioxide sorbent material dewaxes, and degreasing and impurity elimination are rich in supercritical CO Salanesol
2in fluid, the second extraction kettle pressure is 28Mpa, and temperature is 60 ℃;
4) three grades of extractions: the effluent of the second extraction kettle enters in the third extraction kettle with AB-8 resin sorbent, this kind of sorbent material can optionally absorb Salanesol, the third extraction kettle pressure is 25Mpa, temperature is 45 ℃, the tobacco flavor matter that comprises tobacco cleaned oil flowing out from the 3rd extraction kettle carries out separation in separating still, obtain the by product of this invention, for the blending of high-grade cigarette;
5) fractionation by adsorption and recrystallization: it is sherwood oil by volume ratio that extraction finishes rear: the eluent that ethyl acetate is 4:1 carries out wash-out the 3rd extraction kettle, under-18 ℃ of conditions, with sherwood oil, carry out recrystallization afterwards, filter, be dried after recrystallization thing, obtain white flour, through HPLC, detect, the Salanesol purity of extraction is 96%.
Although above-mentioned, the specific embodiment of the present invention is described; but be not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various modifications that creative work can make or distortion still in protection scope of the present invention.
Claims (8)
1. a technique of extracting Salanesol, is characterized in that, comprises the following steps: raw materials pretreatment, one-level extraction, secondary extraction, three grades of extractions, wash-outs obtain Salanesol.
2. the technique of extraction Salanesol as claimed in claim 1, is characterized in that, specifically comprises the following steps:
1) raw materials pretreatment: by drying tobacco, pulverizing;
2) one-level extraction: add the first extraction kettle to carry out the first of Salanesol pretreated raw material and carry, extracting pressure is 28-32Mpa, and temperature is 65-75 ℃, CO
2flow is 10L ∕ h;
3) secondary extraction: the second extraction kettle that the effluent of the first extraction kettle directly enters with the first sorbent material dewaxes, degreasing and impurity elimination, the second extraction kettle pressure is 26-28Mpa, temperature is 60-70 ℃;
4) three grades of extractions: the effluent of the second extraction kettle enters in the 3rd extraction kettle with the second sorbent material, and described the second sorbent material can optionally absorb Salanesol, and the 3rd extraction kettle pressure is 23-25Mpa, and temperature is 45-60 ℃;
5) recrystallization after wash-out: carry out wash-out, recrystallization after extraction finishes.
3. the technique of extraction Salanesol as claimed in claim 2, is characterized in that, described the first sorbent material is molecular sieve, aluminium sesquioxide or gac.
4. the technique of extraction Salanesol as claimed in claim 2, is characterized in that, described the second sorbent material is chromatography silica gel or resin.
5. the technique of extraction Salanesol as claimed in claim 2, is characterized in that, described in be dried to water content and be less than 2%, grinding particle size is 20-40 order.
6. the technique of extraction Salanesol as claimed in claim 2, is characterized in that, described step 5) middle wash-out is for using the mixture of sherwood oil and ethyl acetate, and volume ratio is 3.5:0.5-1.5.
7. the technique of extraction Salanesol as claimed in claim 2, is characterized in that, described step 5) in recrystallization under-10--25 ℃ condition, with sherwood oil, carry out.
8. the Salanesol obtaining as the technique of the extraction Salanesol of claim 1-7 as described in arbitrarily.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410250187.0A CN104072336B (en) | 2014-06-06 | 2014-06-06 | A kind of technique extracting Salanesol |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410250187.0A CN104072336B (en) | 2014-06-06 | 2014-06-06 | A kind of technique extracting Salanesol |
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| CN104072336A true CN104072336A (en) | 2014-10-01 |
| CN104072336B CN104072336B (en) | 2015-09-30 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114249632A (en) * | 2021-12-20 | 2022-03-29 | 贵州省烟草公司遵义市公司 | Novel process for purifying solanesol based on chemically modified diatomite |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52139711A (en) * | 1976-05-17 | 1977-11-21 | Nisshin Flour Milling Co Ltd | Extraction of solanesole |
| CN1676502A (en) * | 2004-04-03 | 2005-10-05 | 杨群力 | Solanesol refining method |
| CN101497557A (en) * | 2009-03-23 | 2009-08-05 | 西北师范大学 | Method for extracting purified solanesol from potato leaf |
-
2014
- 2014-06-06 CN CN201410250187.0A patent/CN104072336B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52139711A (en) * | 1976-05-17 | 1977-11-21 | Nisshin Flour Milling Co Ltd | Extraction of solanesole |
| CN1676502A (en) * | 2004-04-03 | 2005-10-05 | 杨群力 | Solanesol refining method |
| CN101497557A (en) * | 2009-03-23 | 2009-08-05 | 西北师范大学 | Method for extracting purified solanesol from potato leaf |
Non-Patent Citations (2)
| Title |
|---|
| 王青豪 等: "微波辐射从烟草下脚料中提取茄尼醇", 《化工时刊》 * |
| 王青豪 等: "微波辐射从烟草下脚料中提取茄尼醇", 《化工时刊》, vol. 20, no. 10, 10 October 2006 (2006-10-10), pages 3 - 5 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114249632A (en) * | 2021-12-20 | 2022-03-29 | 贵州省烟草公司遵义市公司 | Novel process for purifying solanesol based on chemically modified diatomite |
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| CN104072336B (en) | 2015-09-30 |
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