CN1030078C - Freezing vacuum extracting method for matrine - Google Patents
Freezing vacuum extracting method for matrine Download PDFInfo
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- CN1030078C CN1030078C CN 91111707 CN91111707A CN1030078C CN 1030078 C CN1030078 C CN 1030078C CN 91111707 CN91111707 CN 91111707 CN 91111707 A CN91111707 A CN 91111707A CN 1030078 C CN1030078 C CN 1030078C
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- matrine
- kuh
- seng
- hot water
- extraction
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- Expired - Fee Related
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Abstract
The present invention relates to a method for extracting matrine from radix sophorae flavescentis. Extraction methods in the past adopt decoction in hot water, and therefore, the extraction methods have the disadvantages of complicated technology, long operation time and high cost. In the method, decoction in hot water is changed into extraction in cold water on the basis of the characteristic that the solubility of matrine in cold water is larger than the solubility of the matrine in hot water, and a certain vacuum degree is maintained; then, the extraction solution is treated through percolation, concentration, hydrogenation, chromatography and salting out to prepared pure matrine. The method has the advantages of simplicity, rapidity, high output rate and good quality.
Description
The present invention relates to a kind of from kuh-seng the method for extracting effective components matrine.
Matrine is a kind ofly to extract from kuh-seng, the Chinese medicine preparation that the treatment hepatopathy is had good result.At present, adopt the hot water extraction method both at home and abroad usually, promptly earlier kuh-seng is pulverized, boiling three times, 2～3 hours first, 1～2 hour for the second time, 1 hour for the third time, collecting amount was equivalent to the extracting solution of 3～5 times of kuh-seng amounts, was condensed into to become 1: 1 fluid extract with the kuh-seng amount, add then and be equivalent to fluid extract amount triple ethanol, stir, staticly settled 12～24 hours, ethanol is reclaimed in distillation, the ethanol that adds triplication is again handled once by above-mentioned steps, after repeatedly chromatography make purer matrine.In addition, also useful acetate direct extraction method, the sour water percolation, the ion exchange extraction method makes crude product earlier, uses a large amount of reagent again, and by aluminum oxide or silica gel G column chromatography, wash-out concentrates after collecting and makes purer matrine.The common drawback of these methods is complex process, and is long in time limit, the cost height.
The objective of the invention is to find a kind of new extracting method, overcome the shortcoming of prior art, simplify extraction process, the reduction of erection time, reduce extraction cost, improve the quality of products.
Main points of the present invention are to place cold water to leach kuh-seng.Evidence, the matrine solubleness in cold water is greater than the solubleness in the hot water, and a large amount of impurity is on the contrary, the solubleness of the solubleness in hot water in the cold water.According to this specific character, adopt the cold water leaching, with the matrine stripping, other composition is still stayed in the kuh-seng, thereby can obtain comparatively purified matrine.
Rapid, complete for what leaching process was carried out, in leaching process, extracting vacuum to liquid level does not have bubble and produces, and remain under the vacuum tightness and leach, in order to the cloth youth motion of molecule, quicken infiltration, dissolving, diffusion process, to greatest extent matrine composition solution-off is come out.
The kuh-seng alkali lye of collecting is condensed into 1: 1 dope under vacuum and certain temperature, promptly amount of liquid equals the weight of raw material kuh-seng.Under normal temperature, normal pressure, be catalyzer then, carry out shortening, make the component and the isomer that contain unsaturated link(age) in the liquid be converted into matrine, to improve the output and the quality of matrine with palladium carbon.Constantly by the check of point sample chromatography, when waiting point consistent with collection of illustrative plates to occur, i.e. expression reacts completely in reaction process.Then reacted liquid is passed through alumina column chromatography, collect the matrine layer, saltouing with heating separates out the matrine crystallization again, promptly gets the matrine elaboration.
The present invention compared with the prior art, it is simple to have technology, extracts fast productive rate height, the measured advantage of matter.Comparing with hot method, can save time 2/3, reduce reagent 50%, reduce cost about 50%, is the collection of illustrative plates that adopts the matrine that the cold two kinds of methods of heat produce below:
Fig. 1 is a hot water extraction matrine collection of illustrative plates
Fig. 2 is a cold water extraction matrine collection of illustrative plates
Embodiment:
Get the kuh-seng crude drug, be ground into 16～18 order meal, add the refrigerated water of quintuple-3～0 ℃, soak into, vacuumize 600～700mmHg post simultaneously, do not have bubble to liquid level and produce.Remain under the vacuum tightness, leached about 8～12 hours, the beginning diacolation is collected the liquid of filtering that is three times in crude drug approximately.Flow rate control is equivalent to the liquid of crude drug amount about 5% at the per minute diacolation.To filter liquid 60～70 ℃ of temperature, under vacuum tightness 600～700mmHg post, be condensed into 1: 1 dope.Under normal temperature, the normal pressure, add the palladium-carbon catalyst that contains palladium 10% and carry out shortening, and point sample chromatography and standard diagram contrast at any time, when consistent with collection of illustrative plates, stopped reaction.With reaction solution chromatography on alumina column, collect the matrine chromatographic solution then, carry out salting-out crystallization again, promptly get pure matrine product.
Claims (1)
1, a kind of method of extracting matrine from kuh-seng is characterized in that placing cold water to extract kuh-seng, and step is:
(1) kuh-seng is pulverized,
(2) add-3～0 ℃ chilled brine of five times of kuh-sengs, under vacuum tightness 600～700mmHg post, leach,
(3) leaching liquid is carried out diacolation, collecting amount is equivalent to 3 times of kuh-seng amount, at vacuum tightness 600～700mmHg, 1: 1 concentration of 60～70 ℃ of following simmer down tos of temperature adds the palladium-carbon catalyst that contains palladium 10% again and carries out shortening, after reacting completely, last alumina chromatographic column carries out chromatography, collect the matrine chromatographic solution, heat salting-out crystallization at last, be product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91111707 CN1030078C (en) | 1991-12-23 | 1991-12-23 | Freezing vacuum extracting method for matrine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91111707 CN1030078C (en) | 1991-12-23 | 1991-12-23 | Freezing vacuum extracting method for matrine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1073681A CN1073681A (en) | 1993-06-30 |
| CN1030078C true CN1030078C (en) | 1995-10-18 |
Family
ID=4910807
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91111707 Expired - Fee Related CN1030078C (en) | 1991-12-23 | 1991-12-23 | Freezing vacuum extracting method for matrine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1030078C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044475C (en) * | 1996-09-10 | 1999-08-04 | 内蒙古苦参生化集团有限责任公司 | Preparing matrine and matrine oxide from sophora alopecuroide and its producing technology |
| CN104886189A (en) * | 2015-06-19 | 2015-09-09 | 湖北中医药大学 | Plant-sourced pesticide microemulsion and preparation method thereof |
| CN110859890B (en) * | 2019-12-06 | 2022-02-08 | 湖北威仕生物药业股份有限公司 | Eucommia ulmoides waist tonifying mixture and application thereof |
-
1991
- 1991-12-23 CN CN 91111707 patent/CN1030078C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1073681A (en) | 1993-06-30 |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |