CN1515581A - Preparation method of ginkgo leaf extract - Google Patents
Preparation method of ginkgo leaf extract Download PDFInfo
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- CN1515581A CN1515581A CNA031148255A CN03114825A CN1515581A CN 1515581 A CN1515581 A CN 1515581A CN A031148255 A CNA031148255 A CN A031148255A CN 03114825 A CN03114825 A CN 03114825A CN 1515581 A CN1515581 A CN 1515581A
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- folium ginkgo
- preparation
- ginkgo extract
- elutriant
- acetone
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000009429 Ginkgo biloba extract Substances 0.000 title abstract 3
- 235000008100 Ginkgo biloba Nutrition 0.000 claims abstract description 75
- 241000218628 Ginkgo Species 0.000 claims abstract description 74
- 235000011201 Ginkgo Nutrition 0.000 claims abstract description 74
- 239000011347 resin Substances 0.000 claims abstract description 53
- 229920005989 resin Polymers 0.000 claims abstract description 53
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000000284 extract Substances 0.000 claims abstract description 43
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000008213 purified water Substances 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 20
- 239000006228 supernatant Substances 0.000 claims abstract description 20
- 238000010828 elution Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000003480 eluent Substances 0.000 claims abstract description 5
- 239000012141 concentrate Substances 0.000 claims abstract description 4
- 238000001179 sorption measurement Methods 0.000 claims abstract description 4
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims abstract description 3
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 38
- 238000010790 dilution Methods 0.000 claims description 21
- 239000012895 dilution Substances 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 11
- 150000001298 alcohols Chemical class 0.000 claims description 5
- 238000004062 sedimentation Methods 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 238000003811 acetone extraction Methods 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 230000008719 thickening Effects 0.000 claims 1
- 235000019441 ethanol Nutrition 0.000 abstract description 25
- 239000002904 solvent Substances 0.000 abstract description 3
- 230000001476 alcoholic effect Effects 0.000 abstract description 2
- 238000007865 diluting Methods 0.000 abstract 1
- 239000012530 fluid Substances 0.000 abstract 1
- -1 keto-alcohol glycosides Chemical class 0.000 description 34
- 239000003463 adsorbent Substances 0.000 description 31
- 229930182470 glycoside Natural products 0.000 description 17
- 235000007586 terpenes Nutrition 0.000 description 17
- 238000005406 washing Methods 0.000 description 17
- HVQAJTFOCKOKIN-UHFFFAOYSA-N flavonol Natural products O1C2=CC=CC=C2C(=O)C(O)=C1C1=CC=CC=C1 HVQAJTFOCKOKIN-UHFFFAOYSA-N 0.000 description 16
- 235000011957 flavonols Nutrition 0.000 description 16
- 238000003756 stirring Methods 0.000 description 16
- 235000012054 meals Nutrition 0.000 description 15
- 230000008929 regeneration Effects 0.000 description 14
- 238000011069 regeneration method Methods 0.000 description 14
- 238000000034 method Methods 0.000 description 12
- 238000005507 spraying Methods 0.000 description 11
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- MOLPUWBMSBJXER-YDGSQGCISA-N bilobalide Chemical compound O([C@H]1OC2=O)C(=O)[C@H](O)[C@@]11[C@@](C(C)(C)C)(O)C[C@H]3[C@@]21CC(=O)O3 MOLPUWBMSBJXER-YDGSQGCISA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 3
- 239000008399 tap water Substances 0.000 description 3
- 235000020679 tap water Nutrition 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 230000000274 adsorptive effect Effects 0.000 description 2
- 229940095054 ammoniac Drugs 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 235000014347 soups Nutrition 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 244000194101 Ginkgo biloba Species 0.000 description 1
- 235000009827 Prunus armeniaca Nutrition 0.000 description 1
- 244000018633 Prunus armeniaca Species 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 235000001497 healthy food Nutrition 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 230000003859 lipid peroxidation Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- OVARTBFNCCXQKS-UHFFFAOYSA-N propan-2-one;hydrate Chemical compound O.CC(C)=O OVARTBFNCCXQKS-UHFFFAOYSA-N 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
Abstract
The preparation method of ginkgo leaf extract includes the following steps: using aqueous ethyl alcohol or methyl alcohol or acetone to extract ginkgo leaf for several times, taking out extract and concentrating the recovering solvent, diluting concentrate by using water or purified water, cooling below 20 deg.C and settling, taking supernatant fluid and making macroporous resin adsorption, using alcoholic solution to make elution, concentrating eluent under the condition of less than 75 deg.C and drying so as to obtain the invented ginkgo leaf extract.
Description
The invention belongs to the extractive technique of the medicinal composition of natural phant, specifically a kind of preparation method of Folium Ginkgo extract.
Ginkgo is one of the most ancient in the world seeds, be described as " living fossil ", Ginkgo Leaf is a kind of important medicinal, healthy food material, its extract (GBE, Egb, Extract of Ginkgo biloba) has great antioxygenation, can remove free radical superfluous in the organism, sun ends the body lipid peroxidation, enhance immunity power, and function such as delay senility, in recent years, particularly German both at home and abroad, Japan, the U.S., country such as France is to the Chemical Composition in the Ginkgo Leaf, and separation method has carried out a large amount of research, has obtained bigger progress, representative is to prepare Folium Ginkgo extract with solvent-extracted method, as German Sehwabe, the Flaschman pharmaceutical factory is mainly the dried meal of Ginkgo Leaf, 60% acetone extracting, press filtration is with CCl
4Degreasing, the acetone water layer is saturated with sulfate of ammoniac, extracts with methylethylketone, is made into certain density ethanolic soln behind the extracting solution concentrating under reduced pressure, adds an amount of Pb (OH)
2Filter, filtrate is saturated with sulfate of ammoniac again after concentrating, the methylethylketone extraction, and the dry back that concentrates of extracting solution is with dry ginkgo (GBE) extract (seeing German Patent ED2117429.1767098) that gets of the refining reconcentration of ethanol.This kind method, the organic and inorganic chemical mediator of use is many, complex process, the cost height, and easily cause the residual quality that influences product.The production technology of at present domestic Folium Ginkgo extract mainly is to adopt water or alcoholic solvent to extract, again through the mode of macroporous resin adsorption, (Chinese patent application number 94114835.1), but that it extracts yield is low, and extract obtained content is not high yet.
The object of the present invention is to provide the preparation method of the Folium Ginkgo extract of a kind of high extraction yield and high extract active constituent content.
It mainly may further comprise the steps the technical scheme of realization the object of the invention:
(a) Ginkgo Leaf 40%-95% ethanol or 40%-100% methyl alcohol or 40%-100% acetone extraction;
(b) get extracting solution and concentrate recovery ethanol or methyl alcohol or acetone;
(c) concentrated solution dilution cooling-sedimentation;
(d) supernatant liquor advances the absorption of styrene tyle macroporous adsorption resin post;
(e) with alcohols or acetone soln wash-out;
(f) elutriant concentrating under reduced pressure drying.
The described concentrated solution thinner of step in aforesaid method (c) can be water or purified water;
Can be at the cooling temperature described in the aforesaid method below 20 ℃, more than-1 ℃;
Described in the step in aforesaid method (a) is to extract with dipping, carries out at a certain temperature, and temperature range can be got normal temperature to 80 ℃;
Step in aforesaid method (c) also can be concentrated solution dilution back roughing out, redilution, cooling natural subsidence;
Step in aforesaid method (e) can also adopt type of elution one time, and eluant strength can be 30%-95%;
Step in aforesaid method (e) can adopt the gradient elution mode, and the concentration control of eluent once can be 0%-30%; Can be 40%-95% for the second time;
Step in aforesaid method (f) elutriant concentrating under reduced pressure temperature is less than 75 ℃.
The used medium of the preparation method of a kind of Folium Ginkgo extract of the present invention does not have or does not have substantially objectionable impurities residual, and technology controlling and process is easy, extracts the yield height, and product working substance content height, particularly content of bilobalide height reach more than 3.5% stay in grade.
The present invention is further illustrated below in conjunction with embodiment, but the present invention also is not limited only to the content of embodiment.
Embodiment one:
Get Ginkgo Leaf 100kg, with 12,10,10 times of amounts of 40% ethanol (be meant raw material weight and solvent volume ratio, continuous embodiment is identical therewith).80 ℃ of dippings stir and extract three times, and each 2 hours, emit extracting solution, merging is concentrated into small volume, adds the water dilution of 5 times of amounts, and soup adds the purified water of 5 times of amounts again at 0 ℃ or-1 ℃ of following standing sedimentation after roughing out.Get supernatant liquor and cross styrene type AB-8 macroporous adsorbent resin, with the washing of 2 times of resin volumes, behind 20% ethanol elution, resin is used 70% ethanol elution again, collect elutriant.Reusable after the resin regeneration.The elutriant concentrating under reduced pressure, drying under reduced pressure then, controlled temperature≤75 ℃, the apricot yellow keto-alcohol glycosides 26.5% of argentiferous, Folium Ginkgo terpene lactones 8.5%, wherein bilobalide is up to 4.2% Folium Ginkgo extract 2.4kg.
Embodiment two:
Get Ginkgo Leaf 200kg and be ground into meal, with 10,6,5 times of amounts of 75% ethanol, 70 ℃ of lixiviates three times, each 3 hours, emit vat liquor, merging is concentrated into small volume, add the purified water dilution of 8 times of amounts, soup adds purified water again and is settled to 1600L after roughing out, in 20 ℃ of standing sedimentations of temperature.Get supernatant liquor and cross DM-130 type macroporous adsorptive resins (styrene type polymeric adsorbent), with the purifying washing of 2 times of resin volumes, behind 30% ethanol elution, the ethanol elution with 95% is collected elutriant.Reusable after the resin regeneration.Elutriant is less than 75 ℃ of temperature concentrating under reduced pressure, and spraying drying must contain flavonol glycosides 〉=28% then, Folium Ginkgo terpene lactones 〉=9% wherein bilobalide up to 4.5% Folium Ginkgo extract 4.2kg.
Embodiment three:
Getting Ginkgo Leaf 200kg is ground into less than 1cm
2Fragment, with 15,14,13 times of amounts of 40% acetone, 65 ℃ of lixiviates three times, each 3 hours, emit vat liquor, merge and be concentrated into small volume, add the purified water dilution of 8 times of amounts, under 20 ℃, leave standstill.Get supernatant liquor and cross AB-8 type macroporous adsorbent resin (styrene type polymeric adsorbent), with the purifying washing of 2 times of resin volumes, the acetone wash-out with 75% is collected elutriant.Reusable after the resin regeneration.The elutriant concentrating under reduced pressure, spraying drying must contain flavonol glycosides 〉=24% then, the Folium Ginkgo extract 4.6kg of Folium Ginkgo terpene lactones 〉=8%.
Embodiment four:
Get Ginkgo Leaf 200kg, with 16,15,14 times of 40% methyl alcohol, 70 ℃ of lixiviates three times, each 3 hours, emit vat liquor, merge and be concentrated into small volume, add the tap water dilution of 8 times of amounts, under 17 ℃, leave standstill.Get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) DM-130, with the purifying washing of 2 times of resin volumes, the methanol-eluted fractions with 75% is collected elutriant.Reusable after the resin regeneration.Elutriant is at≤75 ℃ of concentrating under reduced pressure, and spraying drying must contain flavonol glycosides 〉=24% then, the Folium Ginkgo extract 5.5kg of Folium Ginkgo terpene lactones 〉=6%.
Embodiment five:
Get Ginkgo Leaf 500kg and be ground into meal, with 8,6,5 times of 85% ethanol, 55 ℃ of stirring and leaching three times, each 3 hours, emit vat liquor, merge and be concentrated into small volume, add the purified water dilution of 12 times of amounts, under 7 ℃, leave standstill.Get behind the supernatant liquid filtering after D101 type macroporous adsorptive resins (styrene type polymeric adsorbent), with the purifying washing of 2 times of resin volumes, ethanol elution, collection elutriant with 75%.Resin is reused with 95% ethanol regeneration back again.Elutriant is at≤75 ℃ of concentrating under reduced pressure, and spraying drying must contain flavonol glycosides 〉=24% then, the Folium Ginkgo extract 13.5kg of Folium Ginkgo terpene lactones 〉=6%.
Embodiment six:
Get Ginkgo Leaf 1000kg and be ground into meal, with 5,3,2 times of 95% ethanol, 60 ℃ of lixiviates three times, each 3 hours, emit vat liquor, merge and be concentrated into small volume, add the purified water dilution of 10 times of amounts, under 10 ℃, leave standstill.Get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) DM-130, with the purifying washing of 2 times of resin volumes, the ethanol elution with 75% is collected elutriant.Resin is reused with 95% ethanol regeneration back again.Elutriant at≤75 ℃ of drying under reduced pressure, must contain flavonol glycosides 〉=24% then at≤75 ℃ of concentrating under reduced pressure, the Folium Ginkgo extract 26kg of Folium Ginkgo terpene lactones 〉=10%.
Embodiment seven:
Get Ginkgo Leaf 1000kg and be ground into meal, with 8,6,5 times of 85% methyl alcohol, stirring at normal temperature lixiviate three times, each 5 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 10 times of amounts, leaves standstill under 10 ℃.Get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) D-101A, with the purifying washing of 2 times of resin volumes, the methanol-eluted fractions with 40% is collected elutriant.Reusable after the resin regeneration.Elutriant at≤75 ℃ of drying under reduced pressure, must contain flavonol glycosides 〉=24% then at≤75 ℃ of concentrating under reduced pressure, the Folium Ginkgo extract 23kg of Folium Ginkgo terpene lactones 〉=6%.
Embodiment eight:
Get Ginkgo Leaf 1000kg and be ground into meal, with 8,6,5 times of 100% methyl alcohol, 50 ℃ of lixiviates three times, each 3 hours, emit vat liquor, merging is concentrated into small volume, adds the tap water dilution of 5 times of amounts, after roughing out, after the tap water that adds 5 times of amounts again stirs evenly, under 8 ℃, leave standstill.Get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) HPD-600, with the purifying washing of 2 times of resin volumes, the ethanol elution with 95% is collected elutriant.Reusable after the resin regeneration.Elutriant at≤75 ℃ of drying under reduced pressure, must contain flavonol glycosides 〉=24% then at≤75 ℃ of concentrating under reduced pressure, the Folium Ginkgo extract 29kg of Folium Ginkgo terpene lactones 〉=6%.
Embodiment nine:
Get Ginkgo Leaf 1000kg and be ground into meal, with 7,6,5 times in 70% acetone, 80 ℃ of lixiviates three times, each 2 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 5 times of amounts, after roughing out, after the purified water that adds 5 times of amounts again stirs evenly, under 2 ℃, leave standstill.Get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) D-140, with the purifying washing of 2 times of resin volumes, the acetone wash-out with 95% is collected elutriant.Reusable after the resin regeneration.Elutriant at≤75 ℃ of drying under reduced pressure, must contain flavonol glycosides 〉=24% then at≤75 ℃ of concentrating under reduced pressure, the Folium Ginkgo extract 27kg of Folium Ginkgo terpene lactones 〉=6%.
Embodiment ten:
Get Ginkgo Leaf 1000kg and be ground into meal, with 12,9,9 times in 85% acetone, stirring at normal temperature lixiviate three times, each 6 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 5 times of amounts, after roughing out, after the purified water that adds 5 times of amounts again stirs evenly, under 10 ℃, leave standstill.Get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) ADS-17, with the purifying washing of 2 times of resin volumes, the acetone wash-out with 40% is collected elutriant.Reusable after the resin regeneration.Elutriant is at≤75 ℃ of concentrating under reduced pressure, and spraying drying must contain flavonol glycosides 〉=24%, the Folium Ginkgo extract 25kg of Folium Ginkgo terpene lactones 〉=6%.
Embodiment 11:
Get Ginkgo Leaf 1000kg and be ground into meal, with 10,8,6 times in 95% acetone, stirring at normal temperature lixiviate three times, each 6 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 5 times of amounts, after roughing out, after the purified water that adds 5 times of amounts again stirs evenly, under 6 ℃, leave standstill.Get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) ADS-16, with the purifying washing of 2 times of resin volumes, the acetone wash-out with 75% is collected elutriant.Reusable after the resin regeneration.Elutriant is at≤75 ℃ of concentrating under reduced pressure, and spraying drying must contain flavonol glycosides 〉=24%, the Folium Ginkgo extract 26kg of Folium Ginkgo terpene lactones 〉=6%.
Embodiment 12:
Get Ginkgo Leaf 1000kg and be ground into meal, with 8,6,6 times in 100% acetone, 60 ℃ of lixiviates three times, each 2 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 5 times of amounts, after roughing out, after the purified water that adds 5 times of amounts again stirs evenly, under 5 ℃, leave standstill.Get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) LSA-20, with the purifying washing of 2 times of resin volumes, the methanol-eluted fractions with 70% is collected elutriant.Reusable after the resin regeneration.Elutriant is at≤75 ℃ of concentrating under reduced pressure, and spraying drying must contain flavonol glycosides 〉=24%, the Folium Ginkgo extract 27kg of Folium Ginkgo terpene lactones 〉=6%.
Embodiment 13:
Get Ginkgo Leaf 1000kg and be ground into meal, with 10,8,6 times of 95% methyl alcohol, stirring at normal temperature lixiviate three times, each 6 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 10 times of amounts, after roughing out, leaves standstill under 10 ℃.Get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) HPD-600, with the purifying washing of 2 times of resin volumes, the acetone wash-out with 40% is collected elutriant.Reusable after the resin regeneration.Elutriant is at≤75 ℃ of concentrating under reduced pressure, and spraying drying must contain flavonol glycosides 〉=24%, the Folium Ginkgo extract 24kg of Folium Ginkgo terpene lactones 〉=6%.
Embodiment 14:
Get Ginkgo Leaf 1000kg and be ground into meal, with 8,8,7 times of 95% industrial alcohols, 50 ℃ of lixiviates three times, each 3 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 5 times of amounts, after roughing out, after the purified water that adds 5 times of amounts again stirs evenly, under 4 ℃, leave standstill.Get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) ADS-17, with the purifying washing of 2 times of resin volumes, the methanol-eluted fractions with 95% is collected elutriant.Reusable after the resin regeneration.Elutriant is at≤75 ℃ of concentrating under reduced pressure, and≤75 ℃ of concentrating under reduced pressure dryings must contain flavonol glycosides 〉=24%, the Folium Ginkgo extract 28kg of Folium Ginkgo terpene lactones 〉=6%.
Embodiment 15:
Get Ginkgo Leaf 1000kg and be ground into meal, with 12,12,10 times of 90% industrial alcohols, 80 ℃ of lixiviates three times, each 2 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 5 times of amounts, after roughing out, after the purified water that adds 5 times of amounts again stirs evenly, under 5 ℃, leave standstill.Get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) HPD-450, with the purifying washing of 2 times of resin volumes, the ethanol elution with 75% is collected elutriant.Elutriant is at≤75 ℃ of concentrating under reduced pressure, and spraying drying must contain flavonol glycosides 〉=24%, the Folium Ginkgo extract 25kg of Folium Ginkgo terpene lactones 〉=6%.
Embodiment 16:
Get Ginkgo Leaf 1000kg and be ground into meal, with 8,6,4 times of 95% medicinal alcohols, stirring at normal temperature lixiviate three times, each 2 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 5 times of amounts, after roughing out, after the purified water that adds 5 times of amounts again stirs evenly, under 3 ℃, leave standstill.Get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) DA101D, with the purifying washing of 2 times of resin volumes, the ethanol elution with 75% is collected elutriant.Elutriant is at≤75 ℃ of concentrating under reduced pressure, and spraying drying must contain flavonol glycosides 〉=24%, the Folium Ginkgo extract 32kg of Folium Ginkgo terpene lactones 〉=6%.
Embodiment 17:
Get Ginkgo Leaf 1000kg and be ground into meal, with 6,5,4 times of edible ethanols, 65 ℃ of lixiviates three times, each 2 hours, emit vat liquor, merging is concentrated into small volume, adds the purified water dilution of 5 times of amounts, after roughing out, after the purified water that adds 5 times of amounts again stirs evenly, under 10 ℃, leave standstill.Get supernatant liquor and cross macroporous adsorbent resin (styrene type polymeric adsorbent) D-101, with the purifying washing of 2 times of resin volumes, the ethanol elution with 80% is collected elutriant.Elutriant is at≤75 ℃ of concentrating under reduced pressure, and spraying drying must contain flavonol glycosides 〉=24%, the Folium Ginkgo extract 29kg of Folium Ginkgo terpene lactones 〉=8%.
Claims (9)
1. the preparation method of a Folium Ginkgo extract, it mainly comprises the following steps:
(a) Ginkgo Leaf 40%-95% ethanol or 40%-100% methyl alcohol or 40%-100% acetone extraction;
(b) get extracting solution and concentrate recovery ethanol or methyl alcohol or acetone;
(c) concentrated solution dilution cooling-sedimentation;
(d) supernatant liquor advances the absorption of styrene tyle macroporous adsorption resin post;
(e) with alcohols or acetone soln wash-out;
(f) elutriant concentrating under reduced pressure drying.
2. the preparation method of Folium Ginkgo extract according to claim 1, it is characterized in that: the described concentrated solution thinner of step (c) is water or purified water.
3. the preparation method of Folium Ginkgo extract according to claim 1 and 2, it is characterized in that: the described cooling temperature of step (c) is below 20 ℃.
4. according to the preparation method of each described Folium Ginkgo extract of claim 1 to 3, it is characterized in that: described eluent is methyl alcohol or ethanol or acetone etc.
5. the preparation method of Folium Ginkgo extract according to claim 4 is characterized in that: step (a) is that dipping extracts, and temperature range is a normal temperature to 80 ℃.
6. the preparation method of Folium Ginkgo extract according to claim 5 is characterized in that: step (c) is concentrated solution dilution back roughing out, redilution, cooling natural subsidence.
7. the preparation method of Folium Ginkgo extract according to claim 6, it is characterized in that: step (e) is a type of elution, and eluant strength is 30%-95%.
8. the preparation method of Folium Ginkgo extract according to claim 6, it is characterized in that: step (e) is the gradient elution mode, and eluent wash-out concentration for the first time is 0%-30%, and eluent wash-out concentration for the second time is 40%-95%.
9. according to the preparation method of claim 7 or 8 described Folium Ginkgo extracts, it is characterized in that: step (f) elutriant thickening temperature is less than 75 ℃.
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| CN101939321A (en) * | 2008-02-07 | 2011-01-05 | 明治制果株式会社 | Manufacturing method and manufacturing device of high-content theobromine composition |
| CN102078342A (en) * | 2010-12-22 | 2011-06-01 | 天津泰阳制药有限公司 | Preparation method of water-soluble ginkgo biloba extract (GBE) |
| CN101175506B (en) * | 2005-05-03 | 2012-06-06 | 威玛舒培博士两合公司 | Method for preparing a ginkgo extract having a reduced content of 4'-o-methyl pyridoxine and/or biflavones |
| CN104095889A (en) * | 2014-07-11 | 2014-10-15 | 神威药业集团有限公司 | Preparation method of ginko biloba extract |
| CN105287657A (en) * | 2015-08-04 | 2016-02-03 | 浙江康恩贝制药股份有限公司 | Ginkgo biloba extract for treating epilepsy and application of ginkgo biloba extract for treating epilepsy |
| CN107616406A (en) * | 2017-11-07 | 2018-01-23 | 何本科 | A kind of method that flavonoids medicine is extracted from ginkgo leaf |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5158770A (en) * | 1989-12-29 | 1992-10-27 | Freund Industrial Co., Ltd. | Aqueous solution containing ginkgo leaf extract |
| CN1116532A (en) * | 1994-08-11 | 1996-02-14 | 邓忠元 | Process for producing extract of gingko leaves |
| CN1048724C (en) * | 1995-11-15 | 2000-01-26 | 庚朋 | Process for extracting total flavone from ginkgo leaf |
| CN1374303A (en) * | 2002-03-26 | 2002-10-16 | 贵州省生化工程中心 | Production process of water soluble ginkgo leaf extractive |
| 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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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101175506B (en) * | 2005-05-03 | 2012-06-06 | 威玛舒培博士两合公司 | Method for preparing a ginkgo extract having a reduced content of 4'-o-methyl pyridoxine and/or biflavones |
| CN100463683C (en) * | 2005-08-15 | 2009-02-25 | 黑龙江省珍宝岛制药有限公司 | A kind of Shuxuening injection preparation and its process |
| CN101939321A (en) * | 2008-02-07 | 2011-01-05 | 明治制果株式会社 | Manufacturing method and manufacturing device of high-content theobromine composition |
| CN102078342A (en) * | 2010-12-22 | 2011-06-01 | 天津泰阳制药有限公司 | Preparation method of water-soluble ginkgo biloba extract (GBE) |
| CN104095889A (en) * | 2014-07-11 | 2014-10-15 | 神威药业集团有限公司 | Preparation method of ginko biloba extract |
| CN104095889B (en) * | 2014-07-11 | 2017-11-28 | 神威药业集团有限公司 | A kind of preparation method of ginkgo biloba p.e |
| CN105287657A (en) * | 2015-08-04 | 2016-02-03 | 浙江康恩贝制药股份有限公司 | Ginkgo biloba extract for treating epilepsy and application of ginkgo biloba extract for treating epilepsy |
| CN107616406A (en) * | 2017-11-07 | 2018-01-23 | 何本科 | A kind of method that flavonoids medicine is extracted from ginkgo leaf |
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| CN100362011C (en) | 2008-01-16 |
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Assignee: Beijing Shuanghe Gaoke Natural Drug Co.,Ltd. Assignor: ZHEJIANG CONBA PHARMACEUTICAL Co.,Ltd. Contract record no.: 2010990000753 Denomination of invention: Method for preparing extractive of ginkgo leaves Granted publication date: 20080116 License type: Common License Open date: 20040728 Record date: 20100917 |
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