CN103664981B - The extracting method of lactone in a kind of gingko - Google Patents
The extracting method of lactone in a kind of gingko Download PDFInfo
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- CN103664981B CN103664981B CN201310630541.8A CN201310630541A CN103664981B CN 103664981 B CN103664981 B CN 103664981B CN 201310630541 A CN201310630541 A CN 201310630541A CN 103664981 B CN103664981 B CN 103664981B
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- C07—ORGANIC CHEMISTRY
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- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/22—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains four or more hetero rings
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Abstract
The present invention relates to a kind of extracting method of gingko activeconstituents, particularly relate to the extracting method of lactone in a kind of gingko, belong to technical field of natural product extraction.Comprise the steps: to get gingko, dry, grind into powder, is added in potassium sulfate solution, stirs, heating, and insulation, lets cool, obtain vat liquor; In vat liquor, add isopropylcarbinol, mix, carry out removal of impurities by macroporous adsorbent resin, permeate is collected; Regulate the pH of permeate, then filter with ultra-filtration membrane, obtain ultrafiltration permeate; In ultrafiltration permeate, add ethyl acetate extract, obtain organic phase; Carry out heating to organic phase to concentrate, crystallisation by cooling, leaches crystallization, dries.The extracting method of bilobalide provided by the invention, eliminates the impurity in vat liquor preferably, and activeconstituents can be made to be extracted better, and product yield is high, purity is high.
Description
Technical field
The present invention relates to a kind of extracting method of gingko activeconstituents, particularly relate to the extracting method of lactone in a kind of gingko, belong to technical field of natural product extraction.
Background technology
Gingko is also known as ginkgo, Gong Sunshuzi.Individual as white as polished jade in almond size look, its taste is sweet, bitter, puckery, and overfeeding easily causes diarrhea.Gingko kernel contains various nutrient elements, except starch, protein, fat, carbohydrate, also containing vitamin c, the trace elements such as riboflavin, carotene, calcium, phosphorus, iron, potassium, magnesium, and the composition such as ginkgoic acid, bilobol, five carbon polysaccharide, fat sterol.There is beneficial lung qi, control to cough and breathe heavily, be only with worm, reduce just, flat chapped wrinkle, protect blood vessel, increase dietary function and the medical effects such as volume of blood flow.
The eighties in 20th century, research finds that bilobalide is the strong antagonist of platelet activation factor (PAF), has significant curative effect for cardiovascular and cerebrovascular diseases, and cause the climax of ginkgo research in the world, major part research is wherein carried out for bilobalide.Bilobalide belongs to diterpene-kind compound.From ginkgo, be separated the diterpenoid-lactone obtained has 8, i.e. bilobalide (ginkgolide) A, B, C, J, M at present.Bilobalide molecule has 12 unique carbon backbone structure, is embedded with a tertiary butyl and six five-rings, comprises a spironane, a tetrahydrofuran (THF) ring and three lactonic rings.
Extracting method mainly includes: 1. solvent method; 2. resin adsorption method; 3. silica gel column chromatography; 4. supercritical fluid extraction etc.But these methods all also exist complicated operation, the problem that yield is low, purity is low.
Summary of the invention
The object of the invention is: the extracting method providing a kind of bilobalide, technical scheme is as follows:
In gingko, an extracting method for lactone, comprises the steps:
1st step, by weight, get gingko 30 ~ 40 parts, dry 3 ~ 6 hours at 100 ~ 120 DEG C, grind into powder, being added to mass concentration is in the potassium sulfate solution 150 ~ 200 parts of 0.5 ~ 1%, stirs, is heated to 50 ~ 60 DEG C, be incubated 2 ~ 4 hours, let cool, obtain vat liquor;
2nd step, in vat liquor, add the isopropylcarbinol of 30 ~ 40 parts, mix, carry out removal of impurities by macroporous adsorbent resin, permeate is collected;
PH to 8.0 ~ 10.0 of the 3rd step, adjustment permeate, then filter with ultra-filtration membrane, obtain ultrafiltration permeate;
4th step, in ultrafiltration permeate, add ethyl acetate 50 ~ 60 parts extract, obtain organic phase;
5th step, organic phase carried out to heating and concentrate, when material liquid volume is reduced to original 30% ~ 50%, crystallisation by cooling, leaches crystallization, dries.
Preferably, the macroporous adsorbent resin in the 2nd step is polystyrene macroporous adsorbent resin.
Preferably, polystyrene type macroporous adsorbent resin refers to HP20 type polystyrene macroporous adsorbent resin.
Preferably, in the 3rd step, be regulate pH by the sodium hydroxide solution of mass concentration 1%.
Preferably, the molecular weight cut-off of the ultra-filtration membrane used in the 3rd step is at 200,000 Da ~ 400,000 Da.
Preferably, the bake out temperature in the 5th step is at 80 ~ 100 DEG C, and drying time is 4 ~ 6 hours.
First the present invention passes through gingko grind into powder, again by potassium sulfate solution lixiviate, active substance is wherein separated out more, the object adding isopropylcarbinol is the character changing feed liquid, and impurity is wherein precipitated, better adsorb by macroporous adsorbent resin, reduce foreign matter content, the object of ultrafiltration is further except the macromole such as Deproteinization, colloid impurity, after active substance being transferred to organic phase by extraction, greatly can improve the purity of product.
beneficial effect
The extracting method of bilobalide provided by the invention, eliminates the impurity in vat liquor preferably, and activeconstituents can be made to be extracted better, and product yield is high, purity is high.
Embodiment
Embodiment 1
1st step, get gingko 30Kg, dry 3 hours at 100 DEG C, grind into powder, being added to mass concentration is in the potassium sulfate solution 150Kg of 0.5%, stirs, is heated to 50 DEG C, is incubated 2 hours, lets cool, obtain vat liquor;
2nd step, in vat liquor, add the isopropylcarbinol of 30Kg, mix, carry out removal of impurities by macroporous adsorbent resin, permeate is collected;
The sodium hydroxide solution of the 3rd step, mass concentration 1% regulates the pH to 8.0 of permeate, then filters with ultra-filtration membrane, obtains ultrafiltration permeate;
4th step, in ultrafiltration permeate, add ethyl acetate 50Kg extract, obtain organic phase;
5th step, organic phase carried out to heating and concentrate, when material liquid volume is reduced to original 30%, crystallisation by cooling, leaches crystallization, dries.
Macroporous adsorbent resin in 2nd step is HP20 polystyrene macroporous adsorbent resin, and the molecular weight cut-off of the ultra-filtration membrane used in the 3rd step is 200,000 DaDa, and the bake out temperature in the 5th step is at 80 DEG C, and drying time is 4 hours.
Extract bilobalide 30g altogether, purity is 93%.
Embodiment 2
1st step, get gingko 40Kg, dry 6 hours at 120 DEG C, grind into powder, being added to mass concentration is in the potassium sulfate solution 200Kg of 1%, stirs, is heated to 60 DEG C, is incubated 4 hours, lets cool, obtain vat liquor;
2nd step, in vat liquor, add the isopropylcarbinol of 40Kg, mix, carry out removal of impurities by macroporous adsorbent resin, permeate is collected;
The sodium hydroxide solution of the 3rd step, mass concentration 1% regulates the pH to 10.0 of permeate, then filters with ultra-filtration membrane, obtains ultrafiltration permeate;
4th step, in ultrafiltration permeate, add ethyl acetate 60Kg extract, obtain organic phase;
5th step, organic phase carried out to heating and concentrate, when material liquid volume is reduced to original 50%, crystallisation by cooling, leaches crystallization, dries.
Macroporous adsorbent resin in 2nd step is HP20 polystyrene macroporous adsorbent resin, and the molecular weight cut-off of the ultra-filtration membrane used in the 3rd step is 400,000 Da, and the bake out temperature in the 5th step is at 100 DEG C, and drying time is 6 hours.
Extract bilobalide 32g altogether, purity is 93%.
Embodiment 3
1st step, get gingko 35Kg, dry 5 hours at 110 DEG C, grind into powder, being added to mass concentration is in the potassium sulfate solution 170Kg of 0.7%, stirs, is heated to 55 DEG C, is incubated 3 hours, lets cool, obtain vat liquor;
2nd step, in vat liquor, add the isopropylcarbinol of 35Kg, mix, carry out removal of impurities by macroporous adsorbent resin, permeate is collected;
The sodium hydroxide solution of the 3rd step, mass concentration 1% regulates the pH to 9.0 of permeate, then filters with ultra-filtration membrane, obtains ultrafiltration permeate;
4th step, in ultrafiltration permeate, add ethyl acetate 55Kg extract, obtain organic phase;
5th step, organic phase carried out to heating and concentrate, when material liquid volume is reduced to original 40%, crystallisation by cooling, leaches crystallization, dries.
Macroporous adsorbent resin in 2nd step is HP20 polystyrene macroporous adsorbent resin, and the molecular weight cut-off of the ultra-filtration membrane used in the 3rd step is 300,000, and the bake out temperature in the 5th step is at 90 DEG C, and drying time is 5 hours.
Extract bilobalide 37g altogether, purity is 95%.
Claims (1)
1. the extracting method of lactone in gingko, is characterized in that, comprise the steps:
1st step, by weight, get gingko 30 ~ 40 parts, dry 3 ~ 6 hours at 100 ~ 120 DEG C, grind into powder, being added to mass concentration is in the potassium sulfate solution 150 ~ 200 parts of 0.5 ~ 1%, stirs, is heated to 50 ~ 60 DEG C, be incubated 2 ~ 4 hours, let cool, obtain vat liquor;
2nd step, in vat liquor, add the isopropylcarbinol of 30 ~ 40 parts, mix, carry out removal of impurities by HP20 type polystyrene macroporous adsorbent resin, permeate is collected;
3rd step, regulated pH to 8.0 ~ 10.0 of permeate by the sodium hydroxide solution of mass concentration 1%, then filter with ultra-filtration membrane, obtain ultrafiltration permeate, the molecular weight cut-off of ultra-filtration membrane is at 200,000 Da ~ 400,000 Da;
4th step, in ultrafiltration permeate, add ethyl acetate 50 ~ 60 parts extract, obtain organic phase;
5th step, organic phase carried out to heating and concentrate, when material liquid volume is reduced to original 30% ~ 50%, crystallisation by cooling, leaches crystallization, dries 4 ~ 6 hours for 80 ~ 100 DEG C.
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| CN201310630541.8A CN103664981B (en) | 2013-12-02 | 2013-12-02 | The extracting method of lactone in a kind of gingko |
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| CN103393671A (en) * | 2013-08-21 | 2013-11-20 | 上海信谊百路达药业有限公司 | Extracting and refining method of ginkgolide |
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| US6174531B1 (en) * | 1997-11-25 | 2001-01-16 | Pharmanex Inc. | Methods of preparation of bioginkgo |
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Effective date of registration: 20210428 Address after: 226300 WuJie central bridge, Tongzhou District, Nantong City, Jiangsu Province Patentee after: Nantong Tongzhou District WuJie agricultural electromechanical management station Address before: 226300, Jiangsu Nantong hi tech Zone, Century Road, No. 788 East Science Park, building of excellence Patentee before: NEOVOLTAIC ENERGY NANTONG Co.,Ltd. |