CN101084936B - Method for preparing ginkgo leaves extraction - Google Patents
Method for preparing ginkgo leaves extraction Download PDFInfo
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- CN101084936B CN101084936B CN 200610014206 CN200610014206A CN101084936B CN 101084936 B CN101084936 B CN 101084936B CN 200610014206 CN200610014206 CN 200610014206 CN 200610014206 A CN200610014206 A CN 200610014206A CN 101084936 B CN101084936 B CN 101084936B
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- ethanol
- extract
- folium ginkgo
- molecular weight
- protective agent
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- 235000008100 Ginkgo biloba Nutrition 0.000 title claims abstract description 44
- 241000218628 Ginkgo Species 0.000 title claims abstract description 42
- 235000011201 Ginkgo Nutrition 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 8
- 238000000605 extraction Methods 0.000 title claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000012528 membrane Substances 0.000 claims abstract description 11
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 9
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 239000003223 protective agent Substances 0.000 claims abstract description 9
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000006228 supernatant Substances 0.000 claims abstract description 5
- 239000012141 concentrate Substances 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000000284 extract Substances 0.000 claims description 24
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 20
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 10
- 229930003268 Vitamin C Natural products 0.000 claims description 10
- 235000019154 vitamin C Nutrition 0.000 claims description 10
- 239000011718 vitamin C Substances 0.000 claims description 10
- 229930003944 flavone Natural products 0.000 claims description 9
- 235000011949 flavones Nutrition 0.000 claims description 9
- -1 terpene lactones Chemical class 0.000 claims description 9
- 235000007586 terpenes Nutrition 0.000 claims description 9
- 150000002213 flavones Chemical class 0.000 claims description 8
- 235000006708 antioxidants Nutrition 0.000 claims description 7
- 230000006837 decompression Effects 0.000 claims description 6
- 238000004064 recycling Methods 0.000 claims description 6
- 229920002521 macromolecule Polymers 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000287 crude extract Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract description 2
- 239000009429 Ginkgo biloba extract Substances 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 210000000582 semen Anatomy 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 238000001816 cooling Methods 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 244000194101 Ginkgo biloba Species 0.000 description 3
- HVAUUPRFYPCOCA-AREMUKBSSA-N 2-O-acetyl-1-O-hexadecyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCCOC[C@@H](OC(C)=O)COP([O-])(=O)OCC[N+](C)(C)C HVAUUPRFYPCOCA-AREMUKBSSA-N 0.000 description 2
- 108010003541 Platelet Activating Factor Proteins 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000002137 ultrasound extraction Methods 0.000 description 2
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002212 flavone derivatives Chemical class 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000001497 healthy food Nutrition 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 208000010110 spontaneous platelet aggregation Diseases 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a preparation method of ginkgo leaf extract which comprises the following step in turn: pulverizing dry ginkgo leaf, extracting with aqueous ethanol, adding antioxidant protective agent, mixing, recoverying ethanol under reduced pressure to give concentrate, adding 1-3 times water, standing, centrifuging or filtering to give supernatant or filtrate, performing second order hyperfiltration sequentially with macromolecular and small molecular hyperfiltration membranes, adding antioxidant protective agent, concentrating under reduced pressure, and drying to give crude extract of ginkgo leaf. The inventive preparation method has rational technique, high extraction yield, and easy accessibility and exceed of international standard, good product quality, and easy industrialization production.
Description
Technical field
The present invention relates to the preparation method of Folium Ginkgo extract.
Background technology
Folium Ginkgo is a kind of important medicinal, healthy food material, its extract (GBE, EGB, Extractor of GinkgoBiloba) has great antioxidation, can remove free radical superfluous in the organism, stop the body lipid peroxidating, improve the immunity of body, slow down aging etc., the terpenoid among the GBE is the jinx of platelet activating factor (PAF), has the platelet aggregation of prevention and thrombosed effect.During the nearly last ten years, countries such as domestic and international particularly Germany, Japan, the U.S. and France have carried out big quantity research to the chemical constituent in the Folium Ginkgo and separation method, pharmacological testing and clinical practice.The GBE quality standard of generally acknowledging in the world is at present: general flavone content 〉=24%, and terpene lactones content 〉=6%, this standard has become the quality standard that world many countries is imported and exported gingko leaf preparation now.But domestic production technology is difficult to reach above-mentioned standard, therefore, need do further to improve to the extracting method of GBE.
Technology contents
The preparation method that the purpose of this invention is to provide the Folium Ginkgo extract that a kind of technology is reasonable, active constituent content is high.
The present invention is implemented by following technical proposals.
Folium Ginkgo extract of the present invention (GBE) preparation method comprises the steps: in order
(1) get dry Folium Ginkgo, pulverize, extract, extract the back and in extracting solution, add anti-oxidant protective agent with aquiferous ethanol, mixing, decompression recycling ethanol gets concentrated solution;
(2) get concentrated solution, add the water of 1~3 times of volume, leave standstill, centrifugal or filtration gets supernatant or filtrate;
(3) get supernatant or filtrate, the ultrafilter membrane with macromolecule and small-molecular weight carries out two-stage ultrafiltering in proper order, gets ultrafiltrate;
(4) get ultrafiltrate, add anti-oxidant protective agent, concentrating under reduced pressure, the concentrate drying promptly gets ginkgo biloba crude extract.
In the described step (1), aquiferous ethanol is 50%~95% ethanol, and the best is 80% ethanol; The method of extracting is that perhaps supersound extraction is 2~4 times 50 ℃~80 ℃ following lixiviates 2~4 times.
In the described step (3), the molecular weight of macromolecule ultrafilter membrane is 80,000~120,000, and the molecular weight of small-molecular weight ultrafilter membrane is 0.8 ten thousand~1.5 ten thousand.
In described step (2) and (4), anti-oxidant protective agent is a vitamin C, and its addition is 0.5%~2%.
The Ginkgo total flavones content of the Folium Ginkgo extract of method for preparing is 30~45%, and Folium Ginkgo terpene lactones content is 6~12%.(Food Science, April in 2002,23 (4): 105), the assay of Folium Ginkgo terpene lactones was referring to document (Chinese Pharmaceutical Journal, in November, 1998,33 (11): 656) referring to document for the assay of Ginkgo total flavones
The present invention compared with prior art; adopt the method for anti-oxidant protective agent and two-stage ultrafiltering; the Ginkgo total flavones content of the GBE of preparation can reach 30~45%; Folium Ginkgo terpene lactones content can reach 6~12%; process is reasonable, and the extraction ratio height reaches and surpasses international standard; good product quality, and can realize suitability for industrialized production.
The specific embodiment
To be easier to understand the present invention with reference to the following example, and provide embodiment and be in order to illustrate the present invention, rather than in order to limit the scope of the invention.
Embodiment one
Get dry Folium Ginkgo, pulverize, cross 20 mesh sieves, with 80% ethanol lixiviate twice, 80% ethanol that adds 9 times of material quantities for the first time is in 70 ℃ of stirring and leaching 2 hours, measures 80% ethanol in 70 ℃ of following stirring and leaching 1.5 hours with 7 times for the second time.Merge alcohol extract twice, to the vitamin C that wherein adds 1%, mixing, decompression recycling ethanol to 1.05~1.10 (60 ℃), and the concentrated solution cooling to the water that wherein adds 2 times of volumes, staticly settled 24 hours, and it is centrifugal to get clear liquid.With centrifugal liquid in proper order with molecular weight be 100,000 and molecular weight be that 10,000 ultrafilter membrane carries out two-stage ultrafiltering, add 0.8% vitamin C in the ultrafiltrate, be evaporated to 1.10~1.15 (60 ℃), concentrated solution.With concentrated solution vacuum drying (60 ℃), get Folium Ginkgo extract.This Folium Ginkgo extract contains Semen Ginkgo total flavones 38%, contains Semen Ginkgo terpene lactones content 9%.
Embodiment two
Get dry Folium Ginkgo, pulverize, cross 20 mesh sieves, with 60% ethanol ultrasonic extraction three times, each 1 hour, add 60% ethanol of 8 times of material quantities for the first time, for the second time with use 5 times of material quantity 60% ethanol for the third time.Merge alcohol extract twice, to the vitamin C that wherein adds 1.2%, mixing, decompression recycling ethanol to 1.05~1.10 (60 ℃), the concentrated solution cooling to the water that wherein adds 1.5 times of volumes, staticly settled 24 hours, filtered.Filtrate in proper order with molecular weight be 120,000 and molecular weight be that 1.5 ten thousand ultrafilter membrane carries out two-stage ultrafiltering, add 1% vitamin C in the ultrafiltrate, be evaporated to 1.10~1.15 (60 ℃), concentrated solution.With concentrated solution vacuum drying (60 ℃), get Folium Ginkgo extract.This Folium Ginkgo extract contains Semen Ginkgo total flavones 34%, contains Semen Ginkgo terpene lactones content 8%.
Embodiment three
Get dry Folium Ginkgo, pulverize, cross 20 mesh sieves, with 85% ethanol lixiviate twice, 85% ethanol that adds 10 times of material quantities for the first time is in 70 ℃ of stirring and leaching 2 hours, measures 85% ethanol in 70 ℃ of following stirring and leaching 1.5 hours with 7 times for the second time.Merge alcohol extract twice, to the vitamin C that wherein adds 1%, mixing, decompression recycling ethanol to 1.05~1.10 (60 ℃), and the concentrated solution cooling to the water that wherein adds 2.5 times of volumes, staticly settled 24 hours, and it is centrifugal to get clear liquid.With centrifugal liquid in proper order with molecular weight be 100,000 and molecular weight be that 0.8 ten thousand ultrafilter membrane carries out two-stage ultrafiltering, add 0.8% vitamin C in the ultrafiltrate, be evaporated to 1.10~1.15 (60 ℃), concentrated solution.With concentrated solution vacuum drying (60 ℃), get Folium Ginkgo extract.This Folium Ginkgo extract contains Semen Ginkgo total flavones 41%, contains Semen Ginkgo terpene lactones content 9%.
Embodiment four
Get dry Folium Ginkgo, pulverize, cross 20 mesh sieves, with 75% ethanol ultrasonic extraction four times, each 0.5 hour, for the first time and add 75% ethanol of 7 times of material quantities for the second time, for the second time with use 5 times of material quantity 75% ethanol for the third time.Merge alcohol extract twice, to the vitamin C that wherein adds 1.1%, mixing, decompression recycling ethanol to 1.05~1.10 (60 ℃), the concentrated solution cooling to the water that wherein adds 2.0 times of volumes, staticly settled 24 hours, filtered.Filtrate in proper order with molecular weight be 80,000 and molecular weight be that 0.8 ten thousand ultrafilter membrane carries out two-stage ultrafiltering, add 1% vitamin C in the ultrafiltrate, be evaporated to 1.10~1.15 (60 ℃), concentrated solution.With concentrated solution vacuum drying (60 ℃), get Folium Ginkgo extract.This Folium Ginkgo extract contains Semen Ginkgo total flavones 42%, contains Semen Ginkgo terpene lactones content 9%.
Claims (1)
1. a Folium Ginkgo extract preparation method comprises the steps: in order
(1) get dry Folium Ginkgo, pulverize, extract, extract the back and in extracting solution, add anti-oxidant protective agent with aquiferous ethanol, mixing, decompression recycling ethanol gets concentrated solution;
(2) get concentrated solution, add the water of 1~3 times of volume, leave standstill, centrifugal or filtration gets supernatant or filtrate;
(3) get supernatant or filtrate, the ultrafilter membrane with macromolecule and small-molecular weight carries out two-stage ultrafiltering in proper order, gets ultrafiltrate;
(4) get ultrafiltrate, add anti-oxidant protective agent, concentrating under reduced pressure, the concentrate drying, promptly;
In the described step (1), aquiferous ethanol is 50%~95% ethanol;
In the described step (1), the method for extraction is that perhaps supersound extraction is 2~4 times 50 ℃~80 ℃ following lixiviates 2~4 times;
In the described step (3), the molecular weight of macromolecule ultrafilter membrane is 80,000~120,000, and the molecular weight of small-molecular weight ultrafilter membrane is 0.8 ten thousand~1.5 ten thousand;
In described step (1) and (4), anti-oxidant protective agent is a vitamin C, and its addition is 0.5%~2%;
The Ginkgo total flavones content of the Folium Ginkgo extract of method for preparing is 30~45%, and Folium Ginkgo terpene lactones content is 6~12%.
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CN101084936B true CN101084936B (en) | 2011-07-13 |
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Families Citing this family (13)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102935100A (en) * | 2012-11-30 | 2013-02-20 | 中国人民解放军兰州军区乌鲁木齐总医院 | Preparation method and applications of queen lagerstroemia folium apocyni veneti general flavones |
CN103055014B (en) * | 2012-12-31 | 2014-09-17 | 青岛华仁技术孵化器有限公司 | Folium ginkgo health product for preventing senile dementia and preparation method thereof |
CN104147054B (en) * | 2014-08-08 | 2019-05-14 | 浙江康恩贝制药股份有限公司 | A kind of ginkgo biloba p.e and its preparation method and application |
CN105687263B (en) * | 2016-03-16 | 2016-10-26 | 浙江新昌天然保健品有限公司 | The preparation technology of water soluble ginkgo leaf extract and water soluble ginkgo leaf extract |
CN105902579A (en) * | 2016-04-19 | 2016-08-31 | 重庆中宝生物制药有限公司 | A hot-water sedimentation process for a ginkgo leaf extract product |
CN106377553A (en) * | 2016-09-04 | 2017-02-08 | 陈雄 | Method for preparing ginkgo flavone through using membrane technology |
CN107318957A (en) * | 2017-08-08 | 2017-11-07 | 合肥润雨农业科技有限公司 | A kind of method for storing and refreshing of capsicum |
CN107467523A (en) * | 2017-08-24 | 2017-12-15 | 合肥市福来多食品有限公司 | A kind of method that ginkgo leaf synergetic hydrolysis albumen maintains Spiced beef shelf life good appearance |
CN107982118A (en) * | 2017-11-27 | 2018-05-04 | 广西协成日用化工有限公司 | A kind of perfumed soap |
CN107699376A (en) * | 2017-11-27 | 2018-02-16 | 广西协成日用化工有限公司 | A kind of liquid detergent |
CN107987989A (en) * | 2017-11-27 | 2018-05-04 | 广西协成日用化工有限公司 | A kind of washing powder |
CN108451987A (en) * | 2018-04-03 | 2018-08-28 | 徐州工程学院 | A method of extraction ginko leaves flavone |
CN116808085A (en) * | 2023-07-31 | 2023-09-29 | 宁波大学科学技术学院 | Method for extracting ginkgo leaf flavone by membrane separation and flavone determination method |
Citations (1)
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CN1379026A (en) * | 2002-04-27 | 2002-11-13 | 贵州省生化工程中心 | Process for preparing gingko leaf extract |
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CN1379026A (en) * | 2002-04-27 | 2002-11-13 | 贵州省生化工程中心 | Process for preparing gingko leaf extract |
Non-Patent Citations (1)
Title |
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于涛等.膜分离技术在提取银杏叶黄酮类化合物中的应用.《无锡轻工大学学报》.2004,第23卷(第6期), * |
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