CN102293790A - High purity ginkgolide composition - Google Patents
High purity ginkgolide composition Download PDFInfo
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- CN102293790A CN102293790A CN2011102096749A CN201110209674A CN102293790A CN 102293790 A CN102293790 A CN 102293790A CN 2011102096749 A CN2011102096749 A CN 2011102096749A CN 201110209674 A CN201110209674 A CN 201110209674A CN 102293790 A CN102293790 A CN 102293790A
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- ginkgolide
- lactone
- semen ginkgo
- ethanol
- bilobalide
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- 239000000203 mixture Substances 0.000 title claims abstract description 15
- 229930184727 ginkgolide Natural products 0.000 title abstract description 7
- 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 claims abstract description 68
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 61
- 235000008100 Ginkgo biloba Nutrition 0.000 claims abstract description 49
- 239000011347 resin Substances 0.000 claims abstract description 30
- 229920005989 resin Polymers 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 239000000243 solution Substances 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000284 extract Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000001179 sorption measurement Methods 0.000 claims abstract description 15
- 238000003795 desorption Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- -1 terpene lactones Chemical class 0.000 claims abstract description 10
- 239000003814 drug Substances 0.000 claims abstract description 9
- 230000036541 health Effects 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000002775 capsule Substances 0.000 claims abstract description 5
- 238000002347 injection Methods 0.000 claims abstract description 5
- 239000007924 injection Substances 0.000 claims abstract description 5
- 238000010992 reflux Methods 0.000 claims abstract description 5
- 241000218628 Ginkgo Species 0.000 claims description 46
- 235000011201 Ginkgo Nutrition 0.000 claims description 46
- 150000002596 lactones Chemical class 0.000 claims description 27
- 210000000582 semen Anatomy 0.000 claims description 27
- 239000012141 concentrate Substances 0.000 claims description 14
- 238000010521 absorption reaction Methods 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 7
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 4
- 230000001476 alcoholic effect Effects 0.000 claims description 4
- 239000000287 crude extract Substances 0.000 claims description 4
- 239000004615 ingredient Substances 0.000 claims description 3
- 239000012752 auxiliary agent Substances 0.000 claims description 2
- 235000019636 bitter flavor Nutrition 0.000 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
- BUBVLQDEIIUIQG-UHFFFAOYSA-N 3,4,5-tris(phenylmethoxy)-6-(phenylmethoxymethyl)oxan-2-one Chemical compound C=1C=CC=CC=1COC1C(OCC=2C=CC=CC=2)C(OCC=2C=CC=CC=2)C(=O)OC1COCC1=CC=CC=C1 BUBVLQDEIIUIQG-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 244000194101 Ginkgo biloba Species 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 235000007586 terpenes Nutrition 0.000 abstract description 4
- 239000004480 active ingredient Substances 0.000 abstract description 2
- 229940079593 drug Drugs 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- SQOJOAFXDQDRGF-WJHVHIKBSA-N ginkgolide B Natural products O=C1[C@@H](C)[C@@]2(O)[C@@H]([C@H](O)[C@]34[C@@H]5OC(=O)[C@]23O[C@H]2OC(=O)[C@H](O)[C@@]42[C@H](C(C)(C)C)C5)O1 SQOJOAFXDQDRGF-WJHVHIKBSA-N 0.000 abstract 2
- AMOGMTLMADGEOQ-FNZROXQESA-N Ginkgolide C Chemical compound O([C@H]1O2)C(=O)[C@H](O)C31[C@]14[C@@H](O)[C@@H]5OC(=O)[C@@H](C)[C@]5(O)[C@@]12C(=O)O[C@@H]4[C@@H](O)[C@H]3C(C)(C)C AMOGMTLMADGEOQ-FNZROXQESA-N 0.000 abstract 1
- 238000007865 diluting Methods 0.000 abstract 1
- FPUXKXIZEIDQKW-MFJLLLFKSA-N ginkgolide A Natural products O=C1[C@H](C)[C@@]2(O)[C@@H](O1)C[C@]13[C@@H]4OC(=O)[C@]21O[C@@H]1OC(=O)[C@H](O)[C@]31[C@@H](C(C)(C)C)C4 FPUXKXIZEIDQKW-MFJLLLFKSA-N 0.000 abstract 1
- AMOGMTLMADGEOQ-DPFZUGDXSA-N ginkgolide C Natural products O=C1[C@@H](C)[C@]2(O)[C@H]([C@H](O)[C@@]34[C@H]5[C@H](O)[C@@H](C(C)(C)C)[C@]63[C@H](O)C(=O)O[C@H]6O[C@@]24C(=O)O5)O1 AMOGMTLMADGEOQ-DPFZUGDXSA-N 0.000 abstract 1
- FPUXKXIZEIDQKW-VKMVSBOZSA-N ginkgolide-a Chemical compound O[C@H]([C@]12[C@H](C(C)(C)C)C[C@H]3OC4=O)C(=O)O[C@H]2O[C@]24[C@@]13C[C@@H]1OC(=O)[C@@H](C)[C@]21O FPUXKXIZEIDQKW-VKMVSBOZSA-N 0.000 abstract 1
- SQOJOAFXDQDRGF-MMQTXUMRSA-N ginkgolide-b Chemical compound O[C@H]([C@]12[C@H](C(C)(C)C)C[C@H]3OC4=O)C(=O)O[C@H]2O[C@]24[C@@]13[C@@H](O)[C@@H]1OC(=O)[C@@H](C)[C@]21O SQOJOAFXDQDRGF-MMQTXUMRSA-N 0.000 abstract 1
- 235000019640 taste Nutrition 0.000 abstract 1
- 229960004756 ethanol Drugs 0.000 description 13
- 239000000047 product Substances 0.000 description 11
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- 230000006837 decompression Effects 0.000 description 4
- 229960000935 dehydrated alcohol Drugs 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 3
- 229930003944 flavone Natural products 0.000 description 3
- 235000011949 flavones Nutrition 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 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
- YXHVCZZLWZYHSA-FPLPWBNLSA-N Ginkgoic acid Chemical compound CCCCCC\C=C/CCCCCCCC1=CC=CC(O)=C1C(O)=O YXHVCZZLWZYHSA-FPLPWBNLSA-N 0.000 description 2
- 108010003541 Platelet Activating Factor Proteins 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 150000002213 flavones Chemical class 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000000144 pharmacologic effect Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 206010048962 Brain oedema Diseases 0.000 description 1
- 208000016192 Demyelinating disease Diseases 0.000 description 1
- 206010012305 Demyelination Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000218791 Ginkgoaceae Species 0.000 description 1
- 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
- 150000001408 amides Chemical class 0.000 description 1
- 230000008485 antagonism Effects 0.000 description 1
- 208000006752 brain edema Diseases 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000001149 cognitive effect Effects 0.000 description 1
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- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 229930004069 diterpene Natural products 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002212 flavone derivatives Chemical class 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 201000001119 neuropathy Diseases 0.000 description 1
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- 208000033808 peripheral neuropathy Diseases 0.000 description 1
- 239000002464 receptor antagonist Substances 0.000 description 1
- 229940044551 receptor antagonist Drugs 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
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a high purity ginkgolide composition which is white powder, tastes slightly bitter, and comprises 10 to 20% of ginkgolide A, 10 to 20% of ginkgolide B, 5 to 15% of ginkgolide C, 30 to 50% of bilobalide and 80 to 95% of total terpene lactones. The high purity ginkgolide composition is prepared through the following steps: with ginkgo biloba used as a raw material, extracting the raw material with an ethanol solution having a mass percentage of 20 to 80% by using heating reflux; recovering ethanol by condensing extracts; separating the condensed extract with a macroporous resin column; carrying out desorption with ethanol; diluting the obtained product in the previous step with water; carrying out adsorption and desorption with a gel type hydrogen-bonded adsorption resin; collecting effluent and stripping liquid; carrying out condensing and drying; dissolving the product obtained in the previous step with ethanol and decoloring the product with active carbon; carrying out condensing and drying. The preparation process for the high purity ginkgolide composition has the advantages of simpleness, reliability, low cost, high yield and no utilization of toxic organic solvents in the whole process, and is an environment-friendly process. Compositions with high purity ginkgolide as an active ingredient can be used in the form of various preparations (capsules, tablets, oral liquid, electuary, powder, injections, etc.) of ginkgolide medicines or health products.
Description
Technical field
The present invention relates to a kind of high-purity Semen Ginkgo lactone and compositions, in particular to the production technology of from Folium Ginkgo, extracting high-purity Semen Ginkgo lactone.
Background technology
Semen Ginkgo (Ginkgo biloba L.) is a kind of important medicinal plants, and Folium Ginkgo is the leaf of Ginkgoaceae plant Ginkgo biloba, and its bitter and puckery flavor, property are put down, and Ginkgo total flavones that it is contained and terpene lactones have important medical value.The seventies in last century, Germany takes the lead in having formulated quality standard, i.e. standard silver Fructus Pruni extract (Ginkgo total flavones 〉=24%, terpene lactones 〉=6% for Semen Ginkgo extrac (being called for short GBE), ginkgoic acid≤10ppm), this standard and then also become the international international standard of Semen Ginkgo extrac.Studies show that further (ginkgolides GK) is active ingredient main in the Folium Ginkgo extract to Folium Ginkgo terpene lactones, is the Diterpenes ester compounds, comprises ginkalide A, B, C, J and M (GKA, GKB, GKC, GKJ, GKM) etc.Bilobalide is as platelet activating factor (the platelet activating factor that generally acknowledges, PAF) receptor antagonist, the pharmacological action of its antagonism PAF is fully confirmed. that anti-PAF activity is the highest in the bilobalide is GKB, is GKA secondly, being GKC once more, is GKJ at last.The nineties in 20th century, Japan has developed the gingko leaf preparation that contains bilobalide, bilobalide, is used for the treatment of demyelination neuropathy, encephalomyelopathy and cerebral edema etc.China is the native place of Semen Ginkgo, and resource accounts for about 70% of the world, and numerous its people but buy external product at high price, provides and the raw material major part of these products is Chinese cheapnesss.Along with the arrival of aging society, increase day by day for defying age, the pharmaceutical requirements that improves cognitive competence.Utilizing the Folium Ginkgo resource, develop the medicine or the health product of super quality and competitive price, will be a major issue that is of value to national economy.
At present, the extracting method report about high-purity Semen Ginkgo lactone also has much wherein most separation and purification researchs that concentrate on ginkalide B and ginkalide A and bilobalide.Nankai University has invented a kind of macroporous resin that adopts and has sent out the method for separating bilobalide, adopt big empty amide resin chromatography, methods such as crystallization prepare high-purity Semen Ginkgo lactone, but lack bilobalide in the resulting high-purity lactone, and bilobalide is the important component of performance nervous system pharmacological action in the bilobalide.Pan sees the method for once having invented a kind of coordination method separation bilobalide, and resin that this method is used need be introduced the so-called part of metal ion, and absorption simultaneously also will be carried out at non-aqueous system, and there are a lot of problems in actual applications in this method.A patent as can be known surplus in the of comprehensive domestic 100, present separation and purification aspect to bilobalide, the separation of internal ester monomer in main each that concentrate, and it is less at the Separation Research of the natural combination high-purity product of lactone in the natural silver Folium Pruni, this patent adopts a kind of simple technology, separate obtaining high-purity natural ratio Ginkgo total lactones, effectively kept the inherent natural attribute of Folium Ginkgo.
Summary of the invention
Purpose of the present invention just is to provide a kind of high-purity Semen Ginkgo lactone composition.Preparation technology of the present invention is simple, reliable.High-purity Semen Ginkgo lactone composition can be used as active component and makes the various preparations of cardiovascular and cerebrovascular vessel and spiritual sacred disease quasi drugs or health product (capsule, tablet, oral liquid, electuary, powder, injection etc.) use.
Purpose of the present invention can realize by following technical scheme:
High-purity Semen Ginkgo lactone provided by the invention is a white powder, mildly bitter flavor, Ginkgo total lactones 〉=80%, ginkalide A content 10-20%, ginkalide B content are 10-20%, and ginkalide C content is 5-15%, content of bilobalide is 30-50%, and total lactone content is 80-95%.
Preparation method is to be raw material with the Folium Ginkgo, with mass fraction is that the lixiviate of 20-80% alcoholic solution reflux is extracted, extracting solution concentrates and reclaims ethanol, crossing macroporous resin column separates, alcohol desorption, reclaim ethanol once more, the direct thin up of gained solution or drying got behind the Semen Ginkgo extrac powder behind the thin up, again by adding gel-type hydrogen bonding adsorption resin, collect effluent, concentrated, dry, dissolve with ethanol, decolorizing with activated carbon concentrate, are drying to obtain high-purity natural ratio bilobalide extract (〉=80%) product.
The step that high-purity Semen Ginkgo lactone preparation method provided by the invention comprises:
1) with the Folium Ginkgo being raw material, is that 70-90 ℃ of reflux lixiviate of 20-80% alcoholic solution extracted each 0.5-3 hour 2 times with mass fraction.Extracting solution concentrates and reclaims ethanol.
2) cross macroporous resin column and separate, the post of adsorption column is directly than being 3-10: 1, and the weight ratio of resin and Folium Ginkgo is 0.5-3: 1, use the 50%-90% alcohol desorption, preferred 50-70%.The absorption and the flow velocity of desorbing be 0.5-3BV/H (BV: bed volume, H: hour), reclaim ethanol once more.
3) the direct thin up of gained solution or drying got behind the Semen Ginkgo extrac powder behind the thin up (concentration is 0.1-20%)), again by adding the gel-type hydrogen bonding adsorption resin adsorption and desorption, the post of adsorption column is directly than being 3-10: 1, collect effluent and stripping liquid, the flow velocity of absorption and desorbing is 0.5-3BV/H.Stripping liquid is the ethanol water of 5%-30%.Preferred 5-10%.
4) concentrate, dry preliminary bilobalide crude extract product.
5) in extract and dehydrated alcohol 1: 20-50 (weight: ratio volume), dissolving bilobalide crude extract, (extract and activated carbon part by weight are 1 to decolorizing with activated carbon: 1-5).
6) concentrate, be drying to obtain white high-purity Semen Ginkgo lactone extract (〉=80%) product.
Used macroporous resin is for being macroporous resin ME-1, FL-2, AB-8 or the D101 of main skeleton with styrene in the described separation process.Described gel-type adsorbent resin is MG-1, MG-2, OU-1.(above resin provides by Tianjin Ourui Biology Technology Co., Ltd.)
Compositions provided by the invention is as effective ingredient with high-purity Semen Ginkgo lactone, being equipped with medicine is to go up the acceptable auxiliary agent to make compositions, and the various preparations (capsule, tablet, oral liquid, electuary, powder, injection etc.) that can be used as bilobalide medicine or health product use.
The present invention does from the source, thereby has guaranteed the stable and controllable of products obtained therefrom quality.Preparation technology is simple, reliable, and cost is low, does not use toxic organic solvent in the process, is a kind of environmentally friendly technology.High-purity Semen Ginkgo lactone is made various preparations (capsule, tablet, oral liquid, electuary, powder, the injection etc.) use that compositions can be used as bilobalide medicine or health product as effective ingredient.
The specific embodiment
Can further specify the present invention below in conjunction with embodiment:
Embodiment 1
Get the adding of 100kg Folium Ginkgo and extract in the still, add 80% ethanol 600L, 70 ℃ are stirred extraction 3h down, emit extracting solution, add 80% ethanol 400L again in extracting still, and 70 ℃ are stirred extraction 2h down, emit extracting solution.Merge extracted twice liquid, decompression recycling ethanol, thin up leave standstill 5h to 400L, filter clear liquid.100L ME-1 macroporous adsorbent resin on the clear liquid (the biological company limited of Tianjin ALLRED), control flow velocity 100L/h, after finishing, absorption uses the 200L pure water rinsing, flow velocity 100L/h, after finishing, flushing uses the alcohol desorption of 300L 70%, collect stripping liquid, decompression recycling ethanol gets fluid extract, adds pure water and is diluted to 800L.100L MG-2 gel-type hydrogen bonding adsorption resin on the diluent (the biological company limited of Tianjin ALLRED), control flow velocity 200L/h, use the alcohol desorption of 200L 5% then, collect effluent and stripping liquid, concentrate drying gets 450g bilobalide crude product, and resin is reused with 70% alcohol flushing 300L regeneration reserve next time.450g bilobalide crude product adds active carbon 675g, insulated and stirred 30min with 45L dehydrated alcohol heating (60 ℃) stirring and dissolving, filter, add active carbon 675g, insulated and stirred 30min in the filtrate again, filter, the filtrate concentrate drying gets white total bilobalide 383g.After testing, ginkalide A content is 15.2%, and ginkalide B content is 16.5%, and ginkalide C content is 10%, and content of bilobalide is 40.3%, and total lactone content is 81.0%.
Embodiment 2
Get the adding of 200kg Folium Ginkgo and extract in the still, add 80% ethanol 1200L, 70 ℃ are stirred extraction 3h down, emit extracting solution, add 80% ethanol 400L again in extracting still, and 70 ℃ are stirred extraction 2h down, emit extracting solution.Merge extracted twice liquid, decompression recycling ethanol, thin up leave standstill 5h to 800L, filter clear liquid.200L D101 macroporous adsorbent resin (Tianjin Ourui Biology Technology Co., Ltd. provides) on the clear liquid, control flow velocity 200L/h, after finishing, absorption uses pure water rinsing 400L, flow velocity 200L/h, after finishing, flushing uses the alcohol desorption of 600L 70%, collect stripping liquid, decompression recycling ethanol gets fluid extract, adds pure water and is diluted to 1600L.200L MG-2 gel-type hydrogen bonding adsorption resin on the diluent (the biological company limited of Tianjin ALLRED), control flow velocity 400L/h, use the alcohol desorption of 400L 5% then, collect effluent and stripping liquid, concentrate drying gets 930g bilobalide crude product, and resin is reused with 70% alcohol flushing 600L regeneration reserve next time.930g bilobalide crude product adds active carbon 1395g, insulated and stirred 30min with 93L dehydrated alcohol heating (60 ℃) stirring and dissolving, filter, add active carbon 1395g, insulated and stirred 30min in the filtrate again, filter, the filtrate concentrate drying gets the total bilobalide 770g of near-white.After testing, ginkalide A content is 18.5%, and ginkalide B content is 19.5%, and ginkalide C content is 12.2%, and content of bilobalide is 44.3%, and total lactone content is 94.5%.
Embodiment 3
(our company produces to get the 1000g Folium Ginkgo extract, general flavone content 25%, total lactone content 7%, add 120L pure water stirring and dissolving, 30L MG-2 gel-type hydrogen bonding adsorption resin on the solution (the biological company limited of Tianjin ALLRED), control flow velocity 30L/h, use the alcohol desorption of 60L 5% then, collect effluent and stripping liquid, concentrate drying gets 140g bilobalide crude product, and resin is reused with 70% alcohol flushing 300L regeneration reserve next time.140g bilobalide crude product adds active carbon 210g, insulated and stirred 30min with 14L dehydrated alcohol heating (60 ℃) stirring and dissolving, filter, add active carbon 210g, insulated and stirred 30min in the filtrate again, filter, the filtrate concentrate drying gets the total bilobalide 120g of near-white.After testing, ginkalide A content is 14.5%, and ginkalide B content is 16.3%, and ginkalide C content is 11.2%, and content of bilobalide is 41.6%, and total lactone content is 83.6%.
Claims (6)
1. a high-purity Semen Ginkgo lactone is characterized in that it is a white powder, mildly bitter flavor, ginkalide A content 10-20%, ginkalide B content are 10-20%, and ginkalide C content is 5-15%, content of bilobalide is 30-50%, and total lactone content is 80-95%.Preparation method is to be raw material with Folium Ginkgo or Semen Ginkgo extrac, with mass fraction is that the lixiviate of 20-80% alcoholic solution reflux is extracted, and extracting solution concentrates and reclaims ethanol, crosses macroporous resin column and separates, alcohol desorption, reclaim ethanol once more, the direct thin up of gained solution or drying got behind the Semen Ginkgo extrac powder behind the thin up, again by adding gel-type hydrogen bonding adsorption resin absorption and desorbing, collect effluent and stripping liquid, concentrated, dry, use decolorizing with activated carbon then, be drying to obtain product.。
2. the preparation method of the described high-purity Semen Ginkgo of claim 1 lactone is characterized in that the step that it comprises:
1) with the Folium Ginkgo being raw material, is that the 20-80% alcoholic solution extracts 2 times in 70-90 ℃ of reflux lixiviate with mass fraction, and each 0.5-3 hour, extracting solution concentrated and reclaims ethanol;
2) cross macroporous resin column and separate, the post of adsorption column is directly than being 3-10: 1, and the weight ratio of resin and Folium Ginkgo is 0.5-3: 1, use the 50%-90% alcohol desorption, preferred 50-70%; The flow velocity of absorption and desorbing is 0.5-3BV/H, reclaims ethanol once more;
3) the direct thin up of gained solution or drying got thin up behind the Semen Ginkgo extrac powder, concentration is 0.1-20%, again by adding gel-type hydrogen bonding adsorption resin absorption and desorbing, the post of adsorption column is directly than being 3-10: 1, collect effluent and stripping liquid, the flow velocity of absorption and desorbing is 0.5-3BV/H; Stripping liquid is the ethanol water of 5%-20%;
4) concentrated, dry, promptly obtain the bilobalide crude extract.
5) (ratio of extract weight and ethanol volume is 1: 10-50), (weight ratio of extract and activated carbon is 1 to the bilobalide crude extract: 1-5) to add decolorizing with activated carbon then with anhydrous alcohol solution.
6) concentrated, dry, promptly get high-purity Semen Ginkgo lactone extract.
3. in accordance with the method for claim 1, it is characterized in that macroporous resin used in the described separation process is for being macroporous resin ME-1, FL-2, AB-8 or the D101 of main skeleton with styrene.
4. in accordance with the method for claim 1, it is characterized in that described gel-type hydrogen bonding adsorption resin is MG-1, MG-2, OU-1.
5. the described high-purity Semen Ginkgo of claim 1 lactone composition, it is characterized in that it be with high-purity Semen Ginkgo lactone composition as effective ingredient, being equipped with medicine is to go up medicine or the health product that the acceptable auxiliary agent is made.
6. the bilobalide medicine made of the compositions of the described high-purity Semen Ginkgo of claim 5 lactone or capsule, tablet, oral liquid, electuary, powder or the injection of health product.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102728096A (en) * | 2012-07-10 | 2012-10-17 | 江苏惠康生物有限公司 | Edulcoration method of ginkgo leaf extraction process |
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| CN102728096A (en) * | 2012-07-10 | 2012-10-17 | 江苏惠康生物有限公司 | Edulcoration method of ginkgo leaf extraction process |
| CN102772452A (en) * | 2012-08-17 | 2012-11-14 | 天津泰阳制药有限公司 | Method for producing ultra-low-acid ginkgo leaf extract |
| CN104922109A (en) * | 2015-05-25 | 2015-09-23 | 黑龙江珍宝岛药业股份有限公司 | High-purity ginkgolide composition and preparation method and application thereof |
| CN108853464A (en) * | 2018-09-26 | 2018-11-23 | 浙江圣博康药业有限公司 | A kind of preparation method of ginkgo-leaf oral liquor |
| CN116115656A (en) * | 2023-01-18 | 2023-05-16 | 华润三九（雅安）药业有限公司 | Method for Simultaneously Extracting Ginkgo Brass and Ginkgolide, Extracted Substance, and Ginkgo Extract Preparation |
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