CN102911244A - Method for extracting gymnemic acid from gymnema sylvestre - Google Patents
Method for extracting gymnemic acid from gymnema sylvestre Download PDFInfo
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- CN102911244A CN102911244A CN2011102188098A CN201110218809A CN102911244A CN 102911244 A CN102911244 A CN 102911244A CN 2011102188098 A CN2011102188098 A CN 2011102188098A CN 201110218809 A CN201110218809 A CN 201110218809A CN 102911244 A CN102911244 A CN 102911244A
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- China
- Prior art keywords
- gymnemic acid
- exchange resin
- extracting
- largeleaf gymnema
- ultrafiltration
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- 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.)
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- 229930183009 gymnemic acid Natural products 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 17
- 241000208253 Gymnema sylvestre Species 0.000 title abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 16
- 239000012528 membrane Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003957 anion exchange resin Substances 0.000 claims abstract description 8
- 238000002425 crystallisation Methods 0.000 claims abstract description 7
- 230000008025 crystallization Effects 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000010992 reflux Methods 0.000 claims abstract description 7
- 238000004042 decolorization Methods 0.000 claims abstract description 3
- 241000208251 Gymnema Species 0.000 claims description 17
- 241000037488 Coccoloba pubescens Species 0.000 claims description 16
- 239000001913 cellulose Substances 0.000 claims description 6
- 229920002678 cellulose Polymers 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000010298 pulverizing process Methods 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 5
- 230000006837 decompression Effects 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 abstract description 9
- 238000010521 absorption reaction Methods 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 238000010828 elution Methods 0.000 abstract 1
- 239000000706 filtrate Substances 0.000 abstract 1
- 239000012466 permeate Substances 0.000 abstract 1
- 238000011112 process operation Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- 239000000470 constituent Substances 0.000 description 4
- 238000000502 dialysis Methods 0.000 description 4
- 238000007598 dipping method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 230000002218 hypoglycaemic effect Effects 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 241000345998 Calamus manan Species 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 206010012601 diabetes mellitus Diseases 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 235000012950 rattan cane Nutrition 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 206010007247 Carbuncle Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010017553 Furuncle Diseases 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 208000031226 Hyperlipidaemia Diseases 0.000 description 1
- 102000004877 Insulin Human genes 0.000 description 1
- 108090001061 Insulin Proteins 0.000 description 1
- 208000008589 Obesity Diseases 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 235000003205 Smilax rotundifolia Nutrition 0.000 description 1
- 240000009022 Smilax rotundifolia Species 0.000 description 1
- 208000004078 Snake Bites Diseases 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- -1 al Species 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 229920001429 chelating resin Polymers 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 208000002925 dental caries Diseases 0.000 description 1
- 230000035619 diuresis Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 201000004792 malaria Diseases 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 235000020824 obesity Nutrition 0.000 description 1
- 210000000496 pancreas Anatomy 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 201000003068 rheumatic fever Diseases 0.000 description 1
- 230000003248 secreting effect Effects 0.000 description 1
- 235000021147 sweet food Nutrition 0.000 description 1
- 235000019605 sweet taste sensations Nutrition 0.000 description 1
- 150000008130 triterpenoid saponins Chemical class 0.000 description 1
- 231100000611 venom Toxicity 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention belongs to the field of natural medicinal chemistry, and discloses a method for extracting gymnemic acid from gymnema sylvestre. The method comprises the steps that: a gymnema sylvestre raw material is crushed; 6-10 times of 30-90% ethanol is added for soak extraction 2-3 times; an extraction liquid is filtered and is subjected to ultrafiltration in an ultrafiltration membrane system; ethanol in a permeate is recovered, and the filtrate is subjected to absorption in anion exchange resin; the material is washed by using deionized water, until the material is colorless; the material is eluted by using 3-6BV 50-80% ethanol solution; active carbon is added fro reflux decolorization; an elution liquid is subjected to reduced-pressure standing crystallization; the material is filtered and dried, such that gymnemic acid is obtained. With the gymnemic acid production method provided by the invention, the process operation is simple, energy consumption is low, product purity is high, and the method is suitable for industrialized productions.
Description
Technical field
The invention belongs to the Natural Medicine Chemistry field, especially relate to a kind of method of from Largeleaf Gymnema, extracting gymnemic acid.
Background technology
Largeleaf Gymnema is asclepiadaceae Gymnema plant, cries again Root of Australian Cowplant, Rhizome of Bock Greenbrier, She Tianjiao, meal spoon rattan, with root and complete stool be used as medicine have clearing heat and detoxicating, the effect of wind-expelling pain-stopping.Be usually used in rheumatic arthritis, carbuncle furuncle poison, venomous snake bite.Largeleaf Gymnema in application among the people for a long time, India is among the people for antitumor, separates malaria, diuresis and hypoglycemic etc.
Gymnemic acid (Gymnemic Acid, GA) is a series of triterpenoid saponins.Its general structure is:
Chinese scholars research finds that gymnemic acid has the effects such as hypoglycemic, anti-dental caries and the reaction of inhibition sweet taste.Can also suppress to eat sweet food desire, suppress health to the absorption of sugar, lowering blood glucose helps to repair the pancreas damaged cell, improves the secretory volume of Regular Insulin.Prevent and treat diabetes and obesity effect.Appear on the market at Japan, US and European as protective foods, the Largeleaf Gymnema compound granules that domestic research is successful and Largeleaf Gymnema oral liquid etc. also have hypoglycemic, reducing blood lipid, can be used for prevention and the treatment of diabetes and hyperlipidaemia.
The existing method of extracting gymnemic acid mostly is Amberlyst process and extraction process.Obtain the gymnemic acid of 60-70% by macroporous resin purification such as document " technical study of absorption with macroporous adsorbent resin and purifying gymnemic acid ", product purity is low.Extraction process adopts n-butanol extraction more, reclaims propyl carbinol difficult.
Summary of the invention
The object of the invention is to overcome defective and the deficiency of prior art, a kind of method of extracting gymnemic acid from Largeleaf Gymnema is provided.
The objective of the invention is to be achieved through the following technical solutions:
A kind of method of from spoon, extracting gymnemic acid in the rattan, it is characterized in that: the Largeleaf Gymnema raw material pulverizing, adding 6-10 times of 30-90% alcohol immersion extracts 2-3 time, extracting solution filters and adds ultrafiltration in the ultrafiltration membrane system, sees through in the liquid Recycled ethanol adding anionite-exchange resin to adsorb, and deionized water wash is colourless, use again 3-6BV50-80% ethanolic soln wash-out, wash-out adds the gac reflux decolour, and crystallization is placed in the destainer decompression, leaches and is drying to obtain gymnemic acid.
Described ultra-filtration membrane is the hollow cellulose ultra-filtration membrane of the 2000-6000 of molecular weight cut-off.
Described anionite-exchange resin is weak base anion-exchange resin, preferred D315 weak base anion-exchange resin.
Positively effect of the present invention: adopt soak at room temperature to extract, energy consumption is low, and impurity is few, is conducive to purifying; Adopt the ultra-filtration membrane removal of impurities, belong to physical method, energy consumption is low; Ultra-filtration membrane and ion exchange resin are combined with, and products obtained therefrom purity is high, and the suitability for industrialized production degree is high.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to the following example.
Embodiment
Embodiment 1:
The Largeleaf Gymnema raw material pulverizing, get 5kg, drop in the small-sized extractor, added the 50kg30% alcohol solution dipping 10 hours, leach liquid and added again the equal-volume solution soaking 8 hours, the hollow cellulose membrane ultrafiltration that adds molecular weight cut-off 2000 after united extraction liquid filters, filter under the normal temperature, add the appropriate amount of deionized water dialysis, collect and see through the liquid Recycled ethanol, concentrated solution adds 3L D315 weak base anion-exchange resin post, after absorption finishes, remove the ionized water washing colourless, get again 18L50% ethanolic soln wash-out effective constituent, collect elutriant and added 1kg gac reflux decolour 1 hour, leach gac, be evaporated to 500ml and place crystallization, leach drying, get 105g, content 92% (UV method).
Embodiment 2:
The Largeleaf Gymnema raw material pulverizing, get 5kg, drop in the small-sized extractor, added the 30kg90% alcohol solution dipping 6 hours, extract 3 times, the hollow cellulose membrane ultrafiltration that adds molecular weight cut-off 6000 after united extraction liquid filters, filter under the normal temperature, add the appropriate amount of deionized water dialysis, collect and see through the liquid Recycled ethanol, concentrated solution adds 3L D315 weak base anion-exchange resin post, after absorption finishes, remove the ionized water washing colourless, get again 9L80% ethanolic soln wash-out effective constituent, collect elutriant and added 800g gac reflux decolour 1 hour, leach gac, be evaporated to 300ml and place crystallization, leach drying, get 113g, content 85% (UV method).
Embodiment 3:
The Largeleaf Gymnema raw material pulverizing, get 10kg, drop in the small-sized extractor, added the 80kg50% alcohol solution dipping 10 hours, leach liquid and added again the equal-volume solution soaking 8 hours, the hollow cellulose membrane ultrafiltration that adds molecular weight cut-off 3000 after united extraction liquid filters, filter under the normal temperature, add the appropriate amount of deionized water dialysis, collect and see through the liquid Recycled ethanol, concentrated solution adds 6L D315 weak base anion-exchange resin post, after absorption finishes, remove the ionized water washing colourless, get again 18L70% ethanolic soln wash-out effective constituent, collect elutriant and added 1.5kg gac reflux decolour 1 hour, leach gac, be evaporated to 500ml and place crystallization, leach drying, get 222g, content 89% (UV method).
Embodiment 4:
The Largeleaf Gymnema raw material pulverizing, get 10kg, drop in the small-sized extractor, added the 80kg60% alcohol solution dipping 10 hours, leach liquid and added again the equal-volume solution soaking 8 hours, the hollow cellulose membrane ultrafiltration that adds molecular weight cut-off 3000 after united extraction liquid filters, filter under the normal temperature, add the appropriate amount of deionized water dialysis, collect and see through the liquid Recycled ethanol, concentrated solution adds 8L D301 weak base anion-exchange resin post, after absorption finishes, remove the ionized water washing colourless, get again 40L60% ethanolic soln wash-out effective constituent, collect elutriant and added 2kg gac reflux decolour 1 hour, leach gac, be evaporated to 600ml and place crystallization, leach drying, get 191g, content 86% (UV method).
Claims (3)
1. method of from Largeleaf Gymnema, extracting gymnemic acid, it is characterized in that: the Largeleaf Gymnema raw material pulverizing, adding 6-10 times of 30-90% alcohol immersion extracts 2-3 time, extracting solution filters and adds ultrafiltration in the ultrafiltration membrane system, sees through in the liquid Recycled ethanol adding anionite-exchange resin to adsorb, and deionized water wash is colourless, use again 3-6BV 50-80% ethanolic soln wash-out, wash-out adds the gac reflux decolour, and crystallization is placed in the destainer decompression, leaches and is drying to obtain gymnemic acid.
2. from Largeleaf Gymnema, extract as claimed in claim 1 the method for gymnemic acid, it is characterized in that described ultra-filtration membrane is the hollow cellulose ultra-filtration membrane of the 2000-6000 of molecular weight cut-off.
3. from Largeleaf Gymnema, extract as claimed in claim 1 the method for gymnemic acid, it is characterized in that described anionite-exchange resin is weak base anion-exchange resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102188098A CN102911244A (en) | 2011-08-02 | 2011-08-02 | Method for extracting gymnemic acid from gymnema sylvestre |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102188098A CN102911244A (en) | 2011-08-02 | 2011-08-02 | Method for extracting gymnemic acid from gymnema sylvestre |
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| Publication Number | Publication Date |
|---|---|
| CN102911244A true CN102911244A (en) | 2013-02-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011102188098A Pending CN102911244A (en) | 2011-08-02 | 2011-08-02 | Method for extracting gymnemic acid from gymnema sylvestre |
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| Country | Link |
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| CN (1) | CN102911244A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106518950A (en) * | 2016-10-21 | 2017-03-22 | 广西中医药大学 | Amyrin cinnamate extract and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1322539A (en) * | 2000-05-08 | 2001-11-21 | 陈文彬 | Diabetes-treating medicine preparing process with Chigenteng vane leaf |
| CN101985459A (en) * | 2010-11-18 | 2011-03-16 | 桂林安和药业有限公司 | Process for extracting greater than or equal to 98% of ursolic acid from loquat leaf |
-
2011
- 2011-08-02 CN CN2011102188098A patent/CN102911244A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1322539A (en) * | 2000-05-08 | 2001-11-21 | 陈文彬 | Diabetes-treating medicine preparing process with Chigenteng vane leaf |
| CN101985459A (en) * | 2010-11-18 | 2011-03-16 | 桂林安和药业有限公司 | Process for extracting greater than or equal to 98% of ursolic acid from loquat leaf |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106518950A (en) * | 2016-10-21 | 2017-03-22 | 广西中医药大学 | Amyrin cinnamate extract and preparation method thereof |
| CN106518950B (en) * | 2016-10-21 | 2018-10-30 | 广西中医药大学 | Amyrin cinnamic acid ester extract and preparation method thereof |
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Addressee: Suzhou Baozetang Medical Technology Co.,Ltd. Han Shuyu Document name: Notification of Passing Preliminary Examination of the Application for Invention |
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Application publication date: 20130206 |