CN1317294C - Preparation method of gynostemma pentaphylia total saponin - Google Patents
Preparation method of gynostemma pentaphylia total saponin Download PDFInfo
- Publication number
- CN1317294C CN1317294C CNB031144705A CN03114470A CN1317294C CN 1317294 C CN1317294 C CN 1317294C CN B031144705 A CNB031144705 A CN B031144705A CN 03114470 A CN03114470 A CN 03114470A CN 1317294 C CN1317294 C CN 1317294C
- Authority
- CN
- China
- Prior art keywords
- raw material
- gypenosides
- ethanol
- macroporous resin
- total
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- 235000002956 Gynostemma pentaphyllum Nutrition 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims description 6
- 240000006509 Gynostemma pentaphyllum Species 0.000 title claims 2
- 239000001397 quillaja saponaria molina bark Substances 0.000 title abstract description 8
- 229930182490 saponin Natural products 0.000 title abstract description 8
- 150000007949 saponins Chemical class 0.000 title abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000011347 resin Substances 0.000 claims abstract description 21
- 229920005989 resin Polymers 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000011010 flushing procedure Methods 0.000 claims abstract description 16
- 238000001179 sorption measurement Methods 0.000 claims abstract description 13
- 238000010828 elution Methods 0.000 claims abstract description 9
- 229930187479 gypenoside Natural products 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- 239000006228 supernatant Substances 0.000 claims abstract description 8
- FBFMBWCLBGQEBU-RXMALORBSA-N (2s,3r,4s,5s,6r)-2-[(2r,3r,4s,5s,6r)-2-[[(3s,5r,6s,8r,9r,10r,12r,13r,14r,17s)-3,12-dihydroxy-4,4,8,10,14-pentamethyl-17-[(2s)-6-methyl-2-[(2s,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyhept-5-en-2-yl]-2,3,5,6,7,9,11,12,13,15,16,17-dodecah Chemical class O([C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(C[C@@H]([C@H]4C(C)(C)[C@@H](O)CC[C@]4(C)[C@H]3C[C@H]2O)O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)C)(C)CC1)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O FBFMBWCLBGQEBU-RXMALORBSA-N 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 20
- 239000003513 alkali Substances 0.000 claims description 8
- 238000005352 clarification Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 abstract description 14
- 238000000605 extraction Methods 0.000 abstract description 13
- 241001065361 Gynostemma Species 0.000 abstract description 12
- 239000012530 fluid Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000012670 alkaline solution Substances 0.000 abstract 2
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 239000000284 extract Substances 0.000 description 11
- 239000002253 acid Substances 0.000 description 5
- 230000001476 alcoholic effect Effects 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 229920006395 saturated elastomer Polymers 0.000 description 5
- 238000004042 decolorization Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 235000012054 meals Nutrition 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 240000003185 Gynostemma laxum Species 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000003862 glucocorticoid Substances 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- ZRBFCAALKKNCJG-UHFFFAOYSA-N gypenoside-XVII Natural products C1CC(C2(CCC3C(C)(C)C(OC4C(C(O)C(O)C(CO)O4)O)CCC3(C)C2CC2O)C)(C)C2C1C(C)(CCC=C(C)C)OC(C(C(O)C1O)O)OC1COC1OC(CO)C(O)C(O)C1O ZRBFCAALKKNCJG-UHFFFAOYSA-N 0.000 description 1
- 230000000147 hypnotic effect Effects 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The present invention proposes a method for preparing gypenosides, which belongs to a chemical engineering technique. The method has the advantages of short technological process, high saponin yield and high saponin purity. The method comprises: gynostemma pentaphylla is used as a raw material; the gynostemma pentaphylla is added to water and boiled for extraction; an extracting solution is filtered and clarified; supernatant fluid is introduced to macroporous resin for adsorption; the column is first flushed by an alkaline solution until effluent is colorless and then by water until the effluent is neutral; 50% to 95% Vol ethanol of which the quantity is 5 to 8 times of that of the raw material is used for elution; ethanol is eliminated, and gypenosides are obtained after drying. In the present invention, HPD macroporous resin is used for adsorption, and an alkaline solution is used for flushing the column; therefore, the extraction ratio of gypenosides reaches 7%, and the purity reaches more than 95%; the present invention reduces the procedures of restoration treatment of a resin column, shortens technological process, increases equipment utilization rate, and reduces production cost at the same time.
Description
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 alkali lye flushing pillar removal of impurities of PH 9-10 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 alkali lye flushing pillar removal of impurities of PH 9-10 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 alkali lye flushing pillar removal of impurities of PH 9-10 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)
- The preparation method of 1 one kinds of total gypenosidess, it is characterized in that: be raw material with the gynostemma pentaphylla, the strand prison is added water boil to be extracted, 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, the ethanol drying that removes ethanol eluate handle the total gypenosides goods.
- The preparation method of 2 total gypenosidess according to claim 1 is characterized in that: macroporous resin adopts the HPD resinoid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031144705A CN1317294C (en) | 2003-01-16 | 2003-01-16 | Preparation method of gynostemma pentaphylia total saponin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031144705A CN1317294C (en) | 2003-01-16 | 2003-01-16 | Preparation method of gynostemma pentaphylia total saponin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1517358A CN1517358A (en) | 2004-08-04 |
| CN1317294C true CN1317294C (en) | 2007-05-23 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB031144705A Expired - Lifetime CN1317294C (en) | 2003-01-16 | 2003-01-16 | Preparation method of gynostemma pentaphylia total saponin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1317294C (en) |
Families Citing this family (7)
| 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 |
| CN104398677B (en) * | 2014-11-10 | 2018-11-16 | 云南谷冠生物科技有限公司 | A kind of tartary buckwheat general flavone and Gynostemma Pentaphyllum compound |
| 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 |
| CN107050095B (en) * | 2017-06-21 | 2020-11-24 | 遵义医科大学 | Preparation method of gypenoside side chain oligosaccharide |
| CN113929723A (en) * | 2021-10-10 | 2022-01-14 | 深圳市真味生物科技有限公司 | Preparation method and application of sweet gynostemma pentaphylla sweetener |
Citations (1)
| 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 |
-
2003
- 2003-01-16 CN CNB031144705A patent/CN1317294C/en not_active Expired - Lifetime
Patent Citations (1)
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| "恩七叶甜"绞股蓝总皂甙提取工艺研究 郑小江，湖北民族学院学报(自然科学版)，第19卷第3期 2001 * |
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| Publication number | Publication date |
|---|---|
| CN1517358A (en) | 2004-08-04 |
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| C14 | Grant of patent or utility model | ||
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Preparation method of gynostemma pentaphylia total saponin Effective date of registration: 20160104 Granted publication date: 20070523 Pledgee: Ankang city credit financing Company limited by guarantee Pledgor: ANKANG PHARMACEUTICAL INSTITUTE OF PEKING University Registration number: 2015610000022 |
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Address after: 725000 No. 6 Pioneering East Road, Ankang High-tech Industrial Development Zone, Shaanxi Province Patentee after: Ankang Innovation Institute of Chinese Pharmaceutical Research Co.,Ltd. Address before: 725000 No. 2 Xing'an East Road, Ankang City, Shaanxi Province Patentee before: ANKANG PHARMACEUTICAL INSTITUTE OF PEKING University |
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Effective date of registration: 20190212 Address after: 725000 No. 6 Pioneering East Road, Ankang High-tech Industrial Development Zone, Shaanxi Province Patentee after: ANKANG BEIYIDA PHARMACEUTICAL CO.,LTD. Address before: 725000 No. 6 Pioneering East Road, Ankang High-tech Industrial Development Zone, Shaanxi Province Patentee before: Ankang Innovation Institute of Chinese Pharmaceutical Research Co.,Ltd. |
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Date of cancellation: 20210111 Granted publication date: 20070523 Pledgee: Ankang city credit financing Company limited by guarantee Pledgor: ANKANG PHARMACEUTICAL INSTITUTE OF PEKING University Registration number: 2015610000022 |
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