CN1473838A - Extracting and refining process for alfalfa saponin and alfalfa saponin preparation - Google Patents

Extracting and refining process for alfalfa saponin and alfalfa saponin preparation Download PDF

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Publication number
CN1473838A
CN1473838A CNA031399223A CN03139922A CN1473838A CN 1473838 A CN1473838 A CN 1473838A CN A031399223 A CNA031399223 A CN A031399223A CN 03139922 A CN03139922 A CN 03139922A CN 1473838 A CN1473838 A CN 1473838A
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China
Prior art keywords
alfalfa
saponin
ethanol
alfalfa saponin
powder
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Pending
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CNA031399223A
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苏云驰
徐建平
余从洪
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ZHONGJIAN MEDICINE INST ZHONGSHAN CITY
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ZHONGJIAN MEDICINE INST ZHONGSHAN CITY
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Priority to CNA031399223A priority Critical patent/CN1473838A/en
Publication of CN1473838A publication Critical patent/CN1473838A/en
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Abstract

The extraction and refining process of alfalfa saponin includes cutting dry alfalfa, thrice ethanol reflux extractions, filtering and concentrating to obtain primary concentrated liquid; ethanol precipitation and concentrating supernatant to obtain secondary concentrated liquid; spray drying or vacuum drying the secondary concentrated liquid and sieving to obtain alfalfa saponin extractive. The said process of extracting, separating and refining alfalfa saponin is simple, low in cost and high in yield. Alfalfa saponin has few toxicity and obvious functions of lowering cholesterin and lowering blood fat and may be used in treating atherosclerosis.

Description

The extraction of alfalfa saponin and process for purification and alfalfa saponin preparation
The present invention relates to the preparation of a kind of traditional Chinese medicine extraction method and process for purification and extract.
Clover, the formal name used at school alfalfa is per nnial herb.Use as herbage always.In recent years find that it has good efficacy to hypercholesterolemia, atherosclerosis and hyperlipidemia etc.Pharmaceutical chemistry research shows that also the main component that plays above-mentioned effect is an alfalfa saponin.Therefore the method for research extraction alfalfa saponin from clover has important meaning to development and use and the pharmacy aspect of clover.
The purpose of this invention is to provide a kind of method of from clover, extracting alfalfa saponin, from clover, to obtain the alfalfa saponin crude extract.
Another object of the present invention provides a kind of process for purification of alfalfa saponin, to make purer alfalfa saponin from the alfalfa saponin crude extract.
The 3rd purpose of the present invention is that alfalfa saponin crude extract or highly finished product are made formulations such as capsule, tablet, granule and oral liquid.
The general planning of extracting method of the present invention is: get alfalfa hay, chopping, with ethanol (concentration 30%~60%) refluxing extraction three times, wherein consumption of ethanol is: clover: ethanol is 1: 8~12 for the first time, is 1: 6~10 for the second time, is 1: 4~8 for the third time.United extraction liquid filters, and filtrate recycling ethanol concentrates, and gets once concentration liquid.Once concentration liquid is handled by one of following two kinds of methods:
1. once concentration liquid adds 95% ethanol, reaches 65%~85% to alcohol concn, stirs evenly, and leaves standstill 12~48 hours, abandons precipitation, and supernatant liquor reclaims ethanol, secondary concentration liquid.
2. once concentration liquid adds in the macroporous resin column absorption (consumption is the clover grass: macroporous resin=4~7: 1), (water consumption is a macroporous resin to elder generation's water wash-out: water=1: 4~8), abandon water liquid, use 55~75% ethanol elutions (macroporous resin: ethanol=1: 4~8) again, collect ethanol eluate, reclaim ethanol, get secondary concentration liquid.The big pore resin is the commercially available universal product.
At last,, sieve, get the total saponin of alfalfa crude extract spraying of secondary concentration liquid or vacuum-drying.
Obtain the total saponin of alfalfa crude extract, can be used to make various clinical administration formulations.Also can it is further refining, process for purification is as follows:
With above-mentioned gained secondary concentration liquid or gained dry powder (being crude extract), add methyl alcohol or ether or propyl carbinol solvent, extraction or backflow, wherein the consumption of solvent is the clover grass: solvent=1: 1~3), 3~6 hours time.Waste, solvent recuperation gets concentrated solution, and spraying or vacuum-drying must be made with extra care total saponin of alfalfa.
Slightly carry powder or refined powder with what aforesaid method made, add auxiliary material necessary on the technology of pharmaceutics, can make formulations such as capsule, tablet, granule and oral liquid respectively.
The invention has the advantages that: 1. the method for this extraction, separation, refining alfalfa saponin, technology is simple, ripe, and laboratory and big production all are suitable for.Extraction cost is low, the yield height.2. according to toxicity, general pharmacology and results of pharmacodynamic test, several nontoxicitys of alfalfa saponin, application safety, effect such as decreasing cholesterol, reducing blood-fat significantly, the mechanism uniqueness, study of anti-atherogenic effect is strong.
Provide embodiment below.
Embodiment 1: the extraction of total saponin of alfalfa (crude extract)
Get alfalfa hay 1kg, chopping, with 40% alcohol reflux three times, ethanol consumption 8kg for the first time, time 2h, the second time ethanol consumption 7kg, time 1.5h, ethanol consumption 6kg for the third time, time 1h.United extraction liquid filters waste.Filtrate recycling ethanol gets once concentration liquid.Add 95% ethanol again, about 70% to alcohol concn, stir evenly, standing over night (about 12 hours) is abandoned precipitation.Supernatant liquor reclaims ethanol, gets secondary concentration liquid.Vacuum-drying is sieved, and gets the total saponin of alfalfa crude extract.Yield 4.3%.
Embodiment 2: total saponin of alfalfa refining
Get alfalfa hay 1kg, press the operation of embodiment 1, make total saponins and slightly carry powder.Add 10kg methyl alcohol, backflow 10h abandons precipitation, and the methanol solution ether defatting reclaims methyl alcohol, and concentrated solution gets the refining dry powder 18g of total saponin of alfalfa through vacuum-drying.
Embodiment 3: alfalfa saponin capsule and preparation method thereof I
Get alfalfa saponin and slightly carry powder 860g, starch 400g, 10% starch slurry 60g, mixing is processed into 1000 of capsules.Be used for the treatment of hypercholesterolemia and mixed type hyperlipidemia, every day 3 times, each 2.45 days is a course of treatment.
Embodiment 4: alfalfa saponin capsule and preparation method thereof II
Get total saponin of alfalfa refining dry powder 150g, starch 73g, 10% starch slurry 20g, mixing, be processed into 1000 of capsules.Be used for the treatment of hypercholesterolemia and mixed type hyperlipidemia, every day 3 times, each 2.45 days is a course of treatment.
Embodiment 5: alfalfa saponin sheet and preparation method thereof
Get alfalfa saponin and slightly carry powder 860g or refined powder 150g, add Microcrystalline Cellulose 340g, Magnesium Stearate 10g, mixing is pressed into 1000 on tabletting machine.Be used for the treatment of hypercholesterolemia and mixed type hyperlipidemia, every day 3 times, each 2.45 days is a course of treatment.
Embodiment 6: alfalfa saponin granule and preparation method thereof
Get alfalfa saponin and slightly carry powder 1720g or refined powder 300g, add N.F,USP MANNITOL 600g, 3% Gonak 120g, mixing, granulate, packing is divided into 1000 bags, be used for the treatment of treatment hypercholesterolemia and mixed type hyperlipidemia, every day 3 times, each 1 bag.45 days is a course of treatment.
Embodiment 7: alfalfa saponin oral liquid and preparation method thereof
Get alfalfa saponin refined powder 150g, brown sugar 200g or stevioside 3g water dissolution 5000ml, mixing, homogeneous, packing is divided into 10 bottles, every bottle of 500ml.Be used for the treatment of treatment hypercholesterolemia and mixed type hyperlipidemia, every day 3 times, each 10ml.45 days is a course of treatment.
The invention is not restricted to the foregoing description.According to principle of the present invention and general pharmacy general knowledge, can do suitably to improve to extraction and process for refining; The alfalfa saponin that obtains slightly carries powder or refined powder also can be made other formulation; Every kind of formulation all can be used other auxiliary material instead.These improvement all should comprise in the present invention.

Claims (6)

1. the extracting method of an alfalfa saponin, it is characterized in that comprising the steps: to get alfalfa hay, chopping, with ethanol (concentration 30%~60%) refluxing extraction three times, wherein consumption of ethanol is: clover: ethanol is 1: 8~12 for the first time, being 1: 6~10 for the second time, is 1: 4~8 for the third time; United extraction liquid filters, and filtrate recycling ethanol concentrates, and gets once concentration liquid; Once concentration liquid is by following a, and one of two kinds of methods of b are handled:
A. once concentration liquid adds 95% ethanol, reaches 65%~85% to alcohol concn, stirs evenly, and leaves standstill 12~48 hours, abandons precipitation, and supernatant liquor reclaims ethanol, secondary concentration liquid;
B. once concentration liquid adds in the macroporous resin column absorption (consumption is the clover grass: macroporous resin=4~7: 1), (water consumption is a macroporous resin to elder generation's water wash-out: water=1: 4~8), abandon water liquid, use 55~75% ethanol elutions (macroporous resin: ethanol=1: 4~8) again, collect ethanol eluate, reclaim ethanol, get secondary concentration liquid;
At last,, sieve, get the total saponin of alfalfa crude extract spraying of secondary concentration liquid or vacuum-drying.
2. the process for purification of an alfalfa saponin is characterized in that: after making crude extract by the method for claim 1, add methyl alcohol or ether or propyl carbinol solvent, and extraction or reflux, wherein the consumption of solvent is the clover grass: solvent=1: 1~3), 3~6 hours time; Waste, solvent recuperation gets concentrated solution, and spraying or vacuum-drying must be made with extra care total saponin of alfalfa.
3. alfalfa saponin capsule is characterized in that: slightly carry with alfalfa saponin and make capsule after powder or refined powder add auxiliary material.
4. alfalfa saponin sheet is characterized in that: slightly carry with alfalfa saponin and be pressed into tablet after powder or refined powder add auxiliary material and excipient.
5. alfalfa saponin granule is characterized in that: slightly carry powder or refined powder adds auxiliary material and excipient with alfalfa saponin, make particle.
6. alfalfa saponin oral liquid is characterized in that: slightly carry powder or refined powder is dissolved in water with alfalfa saponin, add auxiliary material, make oral liquid.
CNA031399223A 2003-07-23 2003-07-23 Extracting and refining process for alfalfa saponin and alfalfa saponin preparation Pending CN1473838A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008006224A1 (en) 2006-07-13 2008-01-17 Medicago, Inc Medicagenic acid saponin and uses thereof
CN101912436A (en) * 2010-08-31 2010-12-15 扬州大学 Ultrasonic extraction method of alfalfa saponin
CN102552643A (en) * 2010-12-21 2012-07-11 中山市中健药物研究所有限公司 Combination with blood fat reducing function and application of same

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008006224A1 (en) 2006-07-13 2008-01-17 Medicago, Inc Medicagenic acid saponin and uses thereof
CN101912436A (en) * 2010-08-31 2010-12-15 扬州大学 Ultrasonic extraction method of alfalfa saponin
CN102552643A (en) * 2010-12-21 2012-07-11 中山市中健药物研究所有限公司 Combination with blood fat reducing function and application of same

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