CN1944453A - Method for extracting hemsleyadin - Google Patents
Method for extracting hemsleyadin Download PDFInfo
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- CN1944453A CN1944453A CN 200610011065 CN200610011065A CN1944453A CN 1944453 A CN1944453 A CN 1944453A CN 200610011065 CN200610011065 CN 200610011065 CN 200610011065 A CN200610011065 A CN 200610011065A CN 1944453 A CN1944453 A CN 1944453A
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Abstract
The process of extract hemsleyadin includes the following steps: crushing hemsleya tuber, reflux extracting and filtering to prepare crude extractum; suspending the extractum in hot water, pouring into macroporous adsorbing chromatographic column, eluting and concentrating to prepare crude hemsleyadin product; and final dissolving, crystallization, etc to obtain hemsleyadin product. The present invention has high hemsleya tuber resource utilizing rate, high product quality, low production cost and other advantages.
Description
Technical field
The invention belongs to technical field of plant extraction, be specifically related to a kind of by the method for extracting Hemsleyadin in the hymsleya amabilis plant.
Background technology
Hymsleya amabilis claims largeseed hemsleya root, Qu Lian again, mainly is distributed in mountain area, China southwest.The Hemsleyadin that is rich in the hymsleya amabilis stem tuber has high pharmaceutical use, is Hemsleyadin capsule and the hemsleyadine tablet that main raw material is made with it, the treatment that is mainly used in diseases such as upper respiratory tract infection, bacillary dysentery and enteritis clinically.Owing to have characteristics such as evident in efficacy, that taking dose is little, have no drug resistance, be called as " natural antibiotics ", market demand is huge.
Existing Hemsleyadin extraction process is mainly solvent extration, though this method is easy and simple to handle, the product yield is low, the disposable qualification rate of product is low, unit cost is higher.Study carefully its major cause: (1) hymsleya amabilis stem tuber contains multiple glucoside unit, glucoside, organic acid and sugar, prepares very thickness of gained medicinal extract with extraction using alcohol, uses ethyl acetate extraction again after need adding the hot water dissolving in the technology.Because the extremely difficult dispersion of medicinal extract is wrapped up mutually with water, forms heterogeneous suspended matter.Therefore,, form emulsion easily, influence production schedule on the one hand, introduce other impurity on the other hand easily, reduce effect of extracting with in the process of ethyl acetate extraction.In addition, ethyl acetate is difficult to be penetrated in the suspended matter, can not make the Hemsleyadin extracting and enriching that is wrapped in the suspended matter, therefore usually will extract more than seven times in actual production.Nonetheless, the Hemsleyadin of still having an appointment more than 30% can't extracting and enriching, wastes huge.And meanwhile, excessively excavate owing to secular, the wild resource of hymsleya amabilis very lacks, and raw material supply day is becoming tight.These prices of all having aggravated the Hemsleyadin product are soaring, and the commercially available prod per kilogram has reached 2.5～3.0 ten thousand yuan, has had a strong impact on the production and the operation of enterprise.(2) main component of Hemsleyadin is a Cucurbitacin, accounts for more than 95%, and other contains a small amount of second element (accounting for 5%), so has stipulated the physical chemical characteristics parameter such as fusing point, specific rotation, uptake factor of product in the Hemsleyadin quality of production standard.Owing in ethyl acetate extraction technology, introduce too much impurity, the gained crystallization rate that is up to the standards only is 5% in follow-up Crystallization Procedure, the secondary crystal qualification rate is about 25%, portioned product even need carry out the repeatedly crystallization requirement that just can reach quality standards, and the production cycle is long.Therefore, how to solve the problems referred to above that solvent extration exists, improve Hemsleyadin product yield and disposable qualification rate, shorten the production cycle, reduce product cost, improve the utilization ratio of resource, just become the technical problem that needs to be resolved hurrily in the prior art.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of method of extracting Hemsleyadin is provided, utilize the macroporous adsorbent resin technology, the target component is carried out selective enrichment, improve Hemsleyadin yield and the disposable qualification rate of product.
Purpose of the present invention is achieved by the following technical programs.
A kind of method of extracting Hemsleyadin may further comprise the steps:
(1) it is an amount of to get the hymsleya amabilis stem tuber, is crushed to meal, adds weight and be 2～5 times, concentration expressed in percentage by weight and be 10%～100% alcoholic solution as extraction agent, 40 ℃～100 ℃ following refluxing extraction 2～5 times, and each 0.5～4 hour; United extraction liquid filters, and reclaims pure liquid, obtains proportion and be 0.8～1.1 crude extract, and keeping the medicinal extract temperature is 45 ℃～55 ℃;
(2) get crude extract and add the hot water that weight is 40 ℃～80 ℃ of 1～8 times, temperature, stir suspendible, pour on the macroporous adsorption resin chromatography post, be that 10%～100% alcoholic solution carries out wash-out 2～3 times as eluent to chromatography column with concentration expressed in percentage by weight, collection contains the elutriant of Hemsleyadin, is concentrated into 5%～30% of original solution volume, places 1～24 hour, filter, get the Hemsleyadin crude product;
(3) get Hemsleyadin crude product concentration expressed in percentage by weight be 50%～100% alcoholic solution as solvating agent, under 40 ℃～85 ℃, make it dissolving, place crystallization 1～24 hour, filter, drying promptly gets the Hemsleyadin elaboration.
Wherein, described macroporous adsorbent resin is a kind of in nonpolar, polarity or the ion exchange resin.
The described extraction agent of step (1) can also be a ketone solution.
The described eluent of step (2) can also be a ketone solution, or in 1～9: 9～1 weight part ratio blended alcohol, ketone solution.
The described solvating agent of step (3) can also be ketone, ester or ethereal solution.
Described alcohol is methyl alcohol or ethanol, and ketone is acetone, and ester is an ethyl acetate, and ether is ether.
The present invention is directed to the characteristics of hymsleya amabilis raw material, utilize the macroporous adsorbent resin technology that the conventional solvent extraction process is improved, effectively improved the utilization ratio and the disposable qualification rate of hemsleyadin product of hymsleya amabilis resource, reduced production cost significantly.Its technology is easy, controllability is high, has better market prospect.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail, but they are not limitation of the invention.
Embodiment 1
A kind of method of extracting Hemsleyadin, it is an amount of to get the hymsleya amabilis stem tuber, is crushed to meal, adds 3 times of weight, concentration expressed in percentage by weights and be 100% methanol solution, 80 ℃ of following refluxing extraction 5 times, each 1 hour; United extraction liquid filters, and reclaims pure liquid, obtains proportion and be 0.8～1.1 crude extract, and keeping the medicinal extract temperature is 50 ℃; Getting crude extract, to add 1 times of weight, temperature be 50 ℃ hot water, stir suspendible, pour on the nonpolar macroporous adsorption resin chromatography column, be that 50% methanol solution carries out 3 times of column volumes of wash-out to chromatography column with concentration expressed in percentage by weight, carry out wash-out with 85% methyl alcohol again, collect the elutriant that contains Hemsleyadin, be concentrated into 5% of original solution volume, placed 1 hour, and filtered, get the Hemsleyadin crude product; Get Hemsleyadin crude product concentration expressed in percentage by weight and be 80% methanol solution, make it dissolving under 60 ℃, place crystallization 5 hours, filter, drying promptly gets the Hemsleyadin elaboration.
Embodiment 2
A kind of method of extracting Hemsleyadin, it is an amount of to get the hymsleya amabilis stem tuber, is crushed to meal, adds 5 times of weight, concentration expressed in percentage by weights and be 95% ethanolic soln, 80 ℃ of following refluxing extraction 3 times, each 2 hours; United extraction liquid filters, and reclaims pure liquid, obtains proportion and be 0.8～1.1 crude extract, and keeping the medicinal extract temperature is 50 ℃; Getting crude extract, to add 1.5 times of weight, temperature be 65 ℃ hot water, stir suspendible, pour on the polar macroporous adsorption resin chromatography column, be that 30% ethanolic soln carries out 3 times of column volumes of wash-out to chromatography column with concentration expressed in percentage by weight, carry out wash-out with 95% ethanol again, collect the elutriant that contains Hemsleyadin, be concentrated into 10% of original solution volume, placed 12 hours, and filtered, get the Hemsleyadin crude product; Get Hemsleyadin crude product concentration expressed in percentage by weight and be 95% ethanolic soln, make it dissolving under 80 ℃, place crystallization 12 hours, filter, drying promptly gets the Hemsleyadin elaboration.
Embodiment 3
Repeat embodiment 1 or 2, following distinctive points is arranged: described macroporous adsorbent resin is an ion exchange resin.
Embodiment 4
Repeat embodiment 1 or 2, following distinctive points is arranged: described extraction agent is an acetone soln.
Embodiment 5
Repeat embodiment 1 or 2, following distinctive points is arranged: described eluent is an acetone soln.
Embodiment 6
Repeat embodiment 1 or 2, following distinctive points is arranged: described eluent is weight part ratio blended methyl alcohol, acetone soln in 1: 9.
Embodiment 7
Repeat embodiment 1 or 2, following distinctive points is arranged: described eluent is weight part ratio blended methyl alcohol, acetone soln in 9: 1.
Embodiment 8～10
Repeat embodiment 1 or 2, following distinctive points is arranged: described solvating agent is respectively acetone soln, ethyl acetate solution or diethyl ether solution.
Claims (9)
1, a kind of method of extracting Hemsleyadin comprises the step of following order:
(1) it is an amount of to get the hymsleya amabilis stem tuber, is crushed to meal, adds weight and be 2～5 times, concentration expressed in percentage by weight and be 10%～100% alcoholic solution as extraction agent, 40 ℃～100 ℃ following refluxing extraction 2～5 times, and each 0.5～4 hour; United extraction liquid filters, and reclaims pure liquid, obtains proportion and be 0.8～1.1 crude extract, and keeping the medicinal extract temperature is 45 ℃～55 ℃,
(2) get crude extract and add the hot water that weight is 40 ℃～80 ℃ of 1～8 times, temperature, stir suspendible, pour on the macroporous adsorption resin chromatography post, be that 10%～100% alcoholic solution carries out wash-out 2～3 times as eluent to chromatography column with concentration expressed in percentage by weight, collection contains the elutriant of Hemsleyadin, is concentrated into 5%～30% of original solution volume, places 1～24 hour, filter, get the Hemsleyadin crude product;
(3) get Hemsleyadin crude product concentration expressed in percentage by weight be 50%～100% alcoholic solution as solvating agent, under 40 ℃～85 ℃, make it dissolving, place crystallization 1～24 hour, filter, drying promptly gets the Hemsleyadin elaboration.
2, extracting method according to claim 1 is characterized in that: described macroporous adsorbent resin is a kind of in nonpolar, polarity or the ion exchange resin.
3, extracting method according to claim 1 is characterized in that: the described extraction agent of step 1 is a ketone solution.
4, extracting method according to claim 1 is characterized in that: the described eluent of step 2 is a ketone solution.
5, extracting method according to claim 1 is characterized in that: the described eluent of step 2 is alcohol, ketone solution by 1～9: 9～1 mixed.
6, extracting method according to claim 1 is characterized in that: the described solvating agent of step 3 is ketone, ester or ethereal solution.
7, extracting method according to claim 1 or 5, it is characterized in that: described alcohol is methyl alcohol or ethanol.
8, according to the described extracting method of claim 3～6, it is characterized in that: described ketone is acetone.
9, extracting method according to claim 6 is characterized in that: described ester is an ethyl acetate, and ether is ether.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100110651A CN100387612C (en) | 2006-07-21 | 2006-07-21 | Method for extracting hemsleyadin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100110651A CN100387612C (en) | 2006-07-21 | 2006-07-21 | Method for extracting hemsleyadin |
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| Publication Number | Publication Date |
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| CN1944453A true CN1944453A (en) | 2007-04-11 |
| CN100387612C CN100387612C (en) | 2008-05-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2006100110651A Expired - Fee Related CN100387612C (en) | 2006-07-21 | 2006-07-21 | Method for extracting hemsleyadin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009049439A1 (en) * | 2007-10-19 | 2009-04-23 | Xiane Fan | Preparative method of dihydrocucurbitacin f-25-o-acetate and the use thereof in the manufacture of medicaments for treating cancers |
| CN104059121A (en) * | 2014-06-21 | 2014-09-24 | 云南云药医药研究有限公司 | Preparation method for cucurbitacin and Dihydrocucurbitacin F |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1202119C (en) * | 2002-11-21 | 2005-05-18 | 中国科学院昆明植物研究所 | Hemsleyadine derivative and its preparing method and use as bactericidal agent |
-
2006
- 2006-07-21 CN CNB2006100110651A patent/CN100387612C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009049439A1 (en) * | 2007-10-19 | 2009-04-23 | Xiane Fan | Preparative method of dihydrocucurbitacin f-25-o-acetate and the use thereof in the manufacture of medicaments for treating cancers |
| US20100168451A1 (en) * | 2007-10-19 | 2010-07-01 | Xiane Fan | Preparative method of dihydrocucurbitacin f-25-o-acetate and the use thereof in the manufacture of medicaments for treating cancers |
| CN104059121A (en) * | 2014-06-21 | 2014-09-24 | 云南云药医药研究有限公司 | Preparation method for cucurbitacin and Dihydrocucurbitacin F |
| CN104059121B (en) * | 2014-06-21 | 2016-09-14 | 云南云药医药研究有限公司 | A kind of method preparing cucurbitacin, dihydrocucurbitacin F |
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| Publication number | Publication date |
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| CN100387612C (en) | 2008-05-14 |
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Granted publication date: 20080514 Termination date: 20110721 |