CN1517358A - Preparation method of gynostemma pentaphylia total saponin - Google Patents

Preparation method of gynostemma pentaphylia total saponin Download PDF

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Publication number
CN1517358A
CN1517358A CNA031144705A CN03114470A CN1517358A CN 1517358 A CN1517358 A CN 1517358A CN A031144705 A CNA031144705 A CN A031144705A CN 03114470 A CN03114470 A CN 03114470A CN 1517358 A CN1517358 A CN 1517358A
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total
raw material
preparation
gynostemma pentaphylla
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CN1317294C (en
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徐世明
王远清
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Ankang Beiyida Pharmaceutical Stock Co.Ltd.
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ANKANG RESEARCH INTS OF MEDICINE BEIJING UNIV
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Abstract

A process for preparing the gynostemma pentaphylla saponin from gynostemma pentaphylla includes such steps as decocting in water, filter, clarifying, adsorbing the supernatant by macroreticular resin, flushing with alkaline solution and then with water, eluting with alcohol, removing alcohol and drying. Its advantages are high extracting rate (7%) and purity (more than 95%), simple process and low cost.

Description

A kind of preparation method of total gypenosides
Technical field
The invention belongs to the chemical industry technology, specifically the preparation method of total gypenosides.
Background technology
Herb Gynostemmae Pentaphylli total glycosides has functions such as reducing blood-fat, control glucocorticoid side effect, calmness, hypnosis, treatment white hair, anticancer growth, is widely used in medicine industry and foodstuffs industry.Prior art adopts technologies such as activated carbon method, solvent extration, resin adsorption method to extract usually.Application number is 92101498, it is exactly to adopt resin adsorption method that name is called " production technique of long stalk gynostemma laxum ", the raw material decocting is extracted, decocting liquid adds flocculation agent by polyamide column or in decocting liquid and removes non-saponin class impurity, then by macroporous resin adsorption and ethanol elution, elutriant is again by anion-exchange column, the effluent liquid drying handle finished product.The complex process that the prior art yield is high, the production cost height.The simple saponin yield of technology is low and purity is also low.
Summary of the invention
The present invention is for overcoming the deficiency of prior art, proposes a kind of technical process weak point, saponin yield height, gypenoside preparation method that purity is high.
The scheme that the present invention solves its technical problem is: be raw material with the gynostemma pentaphylla, gynostemma pentaphylla is added water boil extracts, filter extracting solution, clarification, supernatant liquor is fed macroporous resin adsorption, is that the alkali lye flushing pillar of 9-11 is colourless to effluent liquid with pH value, and the water flushing is to neutral again, doubly measure the 50%-95% ethanol elution with raw material 5-8 then, remove the ethanol drying handle the total saponin goods of gang Lan.
The invention has the beneficial effects as follows: the present invention is with HPD class macroporous resin adsorption, and as homemade HPD500 resin, the extraction rate reached that makes total gypenosides is to 2-7%, and purity can reach more than 95%; Adopt alkali lye flushing pillar, both improved the saponin rate of recovery, reduced the manipulation of regeneration operation of resin column again, technical process is shortened, improved plant factor simultaneously, reduce production costs.
Embodiment
The invention will be further described below in conjunction with embodiment:
Embodiment 1
With 100 kilograms of gynostemma pentaphylla is raw material, gynostemma pentaphylla is added water boil extract 3 times, and each buck is respectively 8 times, 6 times and 6 times of gynostemma pentaphylla weight, and extraction time was respectively 2 hours, 1.5 hours and 1.5 hours.United extraction liquid, filter the back and place clarification in 24 hours, supernatant liquor is fed the HPD macroporous resin adsorption, treat that effluent liquid is saturated after, be that the alkali lye flushing pillar of 9-11 is colourless to effluent liquid with pH value, the water flushing is to neutral again, use 70% ethanol elution of 7 times of amounts of raw material then, collect elutriant and decolouring, when reclaiming ethanol to relative density 1.20-1.30 (80 ℃ of surveys), to remove the alcoholic acid fluid extract and get 6.7 kilograms of total gypenosidess in 5 hours in 80 ° of-90 ° of dryings, content is 98.8%.
Embodiment 2
With 100 kilograms of gynostemma pentaphylla is raw material, is ground into meal, extracts 3 times with 20 times of water boils, and extraction time was respectively 1.0 hours, 0.5 hour and 0.5 hour.United extraction liquid, filter the back and place clarification in 24 hours, supernatant liquor is fed the D101 macroporous resin adsorption, treat that effluent liquid is saturated after, colourless with the removal of impurities of the alkali lye of PH9-10 flushing pillar to effluent liquid, the water flushing is to neutral again, use 80% ethanol elution of 6 times of amounts of raw material then, collect elutriant and use the LSI-632 resin decolorization, when reclaiming ethanol to relative density 1.2 (80 ℃ of surveys), to remove the alcoholic acid fluid extract and get 5.6 kilograms of total gypenosidess in 5 hours in 70 ℃ of vacuum-dryings, content is 98.1%.
Embodiment 3
With 100 kilograms of gynostemma pentaphylla is raw material, extracts 3 times with 20 times of water boils, and extraction time was respectively 2 hours, 1.5 hours and 1.5 hours.United extraction liquid, filter the back and place clarification, supernatant liquor is fed the D140 macroporous resin adsorption, treat that effluent liquid is saturated after, colourless with the alkali lye flushing pillar removal of impurities of PH 9-10 to effluent liquid, the water flushing is to neutral again, use 95% ethanol elution of 5 times of amounts of raw material then, collect elutriant and use the LSI-632 resin decolorization, when reclaiming ethanol to relative density 1.2 (80 ℃ of surveys), to remove the alcoholic acid fluid extract and get 4.9 kilograms of total gypenosidess in 5 hours in 60 ℃ of vacuum-dryings, content is 97.8%.
Embodiment 4
With 100 kilograms of gynostemma pentaphylla is raw material, is ground into meal, extracts 3 times with 20 times of water boils, and extraction time was respectively 1 hour, 0.5 hour and 0.5 hour.United extraction liquid, filter the back and place clarification, supernatant liquor is fed the D101B macroporous resin adsorption, treat that effluent liquid is saturated after, colourless with the removal of impurities of the alkali lye of PH9-10 flushing pillar to effluent liquid, the water flushing is to neutral again, use 75% ethanol elution of 7 times of amounts of raw material then, collect elutriant and use the LSI-632 resin decolorization, when reclaiming ethanol to relative density 1.2 (80 ℃ of surveys), to remove the alcoholic acid fluid extract and get 6.0 kilograms of total gypenosidess in 5 hours in 75 ℃ of vacuum-dryings, content is 96.0%.
Embodiment 5
With 100 kilograms of gynostemma pentaphylla is raw material, extracts 3 times with 20 times of water boils, and each water consumption is 8 times, 6 times, 6 times of gynostemma pentaphylla weight, and extraction time was respectively 2 hours, 1.5 hours and 1.5 hours.United extraction liquid, filter the back and place clarification in 24 hours, supernatant liquor is fed the D101 macroporous resin adsorption, treat that effluent liquid is saturated after, colourless with the removal of impurities of the alkali lye of PH9-10 flushing pillar to effluent liquid, the water flushing is to neutral again, use 80% ethanol elution of 6 times of amounts of raw material then, collect elutriant and use the BS-1 resin decolorization, when reclaiming ethanol to relative density 1.2 (80 ℃ of surveys), to remove the alcoholic acid fluid extract and get 6.2 kilograms of total gypenosidess in 5 hours in 70 ℃ of vacuum-dryings, content is 95.6%.

Claims (2)

  1. The preparation method of 1 one kinds of total gypenosidess, it is characterized in that: be raw material with the gynostemma pentaphylla, gynostemma pentaphylla is added water boil extracts, filter extracting solution, clarification feeds macroporous resin adsorption with supernatant liquor, with pH value is that the alkali lye flushing pillar of 9-11 is colourless to effluent liquid, water flushing is doubly measured the 50%-95% ethanol elution with raw material 5-8 then to neutral again, remove the ethanol drying handle the total saponin goods of thigh Lan.
  2. The preparation method of 2 total gypenosidess according to claim 1 is characterized in that: macroporous resin adopts the HPD resinoid.
CNB031144705A 2003-01-16 2003-01-16 Preparation method of gynostemma pentaphylia total saponin Active CN1317294C (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101463062B (en) * 2009-01-15 2011-08-17 西北农林科技大学 Compound separated from Gynostemma pentaphylla total saponin acid hydrolysis products
CN101829180B (en) * 2008-03-31 2011-12-21 北京市科威华食品工程技术有限公司 Gynostemma pentaphyllum soft capsule preparation and preparation method thereof
CN103655673A (en) * 2013-12-24 2014-03-26 湖南麓山天然植物制药有限公司 Compound gingko dropping pill and preparation method thereof
CN104398677A (en) * 2014-11-10 2015-03-11 云南谷冠生物科技有限公司 Compound composition of tartary buckwheat general flavone and gynostemma pentaphylla total saponin
CN107050095A (en) * 2017-06-21 2017-08-18 遵义医学院 A kind of preparation method of gypenoside side chain oligosaccharides
CN107126452A (en) * 2016-02-26 2017-09-05 上海中医药大学附属曙光医院 Gypenosides and preparation method thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1068575A (en) * 1992-03-11 1993-02-03 孙文基 The production technique of long stalk gynostemma laxum

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101829180B (en) * 2008-03-31 2011-12-21 北京市科威华食品工程技术有限公司 Gynostemma pentaphyllum soft capsule preparation and preparation method thereof
CN101463062B (en) * 2009-01-15 2011-08-17 西北农林科技大学 Compound separated from Gynostemma pentaphylla total saponin acid hydrolysis products
CN103655673A (en) * 2013-12-24 2014-03-26 湖南麓山天然植物制药有限公司 Compound gingko dropping pill and preparation method thereof
CN104398677A (en) * 2014-11-10 2015-03-11 云南谷冠生物科技有限公司 Compound composition of tartary buckwheat general flavone and gynostemma pentaphylla total saponin
CN107126452A (en) * 2016-02-26 2017-09-05 上海中医药大学附属曙光医院 Gypenosides and preparation method thereof
CN107050095A (en) * 2017-06-21 2017-08-18 遵义医学院 A kind of preparation method of gypenoside side chain oligosaccharides
CN107050095B (en) * 2017-06-21 2020-11-24 遵义医科大学 Preparation method of gypenoside side chain oligosaccharide

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Denomination of invention: Preparation method of gynostemma pentaphylia total saponin

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