CN103524526B - A kind of isolation and purification method of Bilobalide - Google Patents
A kind of isolation and purification method of Bilobalide Download PDFInfo
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Abstract
The invention discloses a kind of isolation and purification method of Bilobalide. The inventive method comprises the following steps: that (1) prepare ginkgolides enriched substance; (2) anti-phase polymeric adsorbent column chromatography makes Bilobalide crude product; (3) after Bilobalide crude product recrystallization, obtain Bilobalide fine work. The content of bilobalide that the inventive method makes can reach 98%-99%. The filler that the inventive method is used is MCI-GEL or the anti-phase polymeric adsorbent of NM100, has well selectively, can greatly improve the separative efficiency of Bilobalide, and can regeneration, and toxicity is low, use cost is low. Solvent of the present invention is simple and easy to get, and device therefor is conventional equipment, easy and simple to handle, less energy consumption, and production safety, pollution-free, products obtained therefrom purity is high, is suitable for suitability for industrialized production, has larger using value.
Description
Technical field
The present invention relates to the isolation and purification method of medicine, be specifically related to a kind of separation of BilobalidePurification process.
Background technology
The one-tenth of ginkgo leaf is grouped into complexity, includes various active composition, mainly contains in flavones, terpeneEster, also has organic acid, alkyl phenol and alkyl phenolic acid, steroidal compounds, trace element etc. in addition.And medicinal ingredient in ginkgo leaf is mainly Ginkgolides and bilobalide-like substances. At present fromIn ginkgo leaf, main separation obtains diterpenoid-lactone and sesquiterpene lactone, Ginkgolide A. B. C,J, M and Bilobalide. Bilobalide belongs to sesquiterpene lactone, only contains one penta in molecular structureAlkane. Bilobalide has very strong biologically active, has many-sided neuroprotection, comprisesPromote nerve growth, improve senile memory, prevent the generation etc. of senile dementia. Due to silverIn apricot leaf, the content of terpene lactones is extremely low, therefore, obtain having the ginkgolides of high medical valueAnd Bilobalide, must ginkgo leaf or its crude extract be extracted refining again. Document report at presentThe ginkgolides extraction separation method in road mainly contains: solvent extraction method, solvent extraction-chromatographic column is dividedFrom method, means of supercritical extraction partition method, high-speed countercurrent chromatography and SMBC method etc.,Wherein applying maximum is chromatographic column partition method, and filler adopts silica gel, aluminium oxide and anti-phase C18 moreSilicagel column filler etc. Chinese invention patent " from ginkgo leaf, extract separating bilobalide A, B,The method of C, J and bilobalide monomer " (number of patent application 200710050242.1) and " fromIn ginkgo leaf, extract the method for separating bilobalide " (number of patent application 200710050244.0)Middle employing silica gel column chromatography separates gingko with the method for n-hexane-ethyl acetate solvent system wash-outLactone. But the silica gel using in the method can not recycling, also will use in a large number and haveMachine solvent elution, is unfavorable for suitability for industrialized production. Chinese invention patent " Ginkgolide A. B. C,The high efficiency separation and purification method of J and bilobalide monomer " (number of patent application200810046162.3) and " preparation method for separating and purifying of Bilobalide " (number of patent application201210457118.8) in adopt respectively preparative high performance liquid chromatography post and reverse phase silica gel post layerAnalyse and prepare Bilobalide, the shortcoming of the method is that reverse phase silica gel volume containing the sample is little, and methyl alcohol or acetonitrile makeConsumption is large, and process costs is higher, is unfavorable for a large amount of preparations. Thereby, above-mentioned process for purification refineRemain in various defects, can not isolate highly purified Bilobalide to high-efficiency and economic environmental protection, urgentlyTreat further to improve the method for extracting separating bilobalide.
Summary of the invention
Technical problem to be solved by this invention is to overcome above-mentioned weak point, and research and design is dividedEasy from purifying, cost is low, be conducive to environmental protection, is applicable to the Bilobalide of suitability for industrialized productionIsolation and purification method.
The invention provides a kind of isolation and purification method of Bilobalide.
Method of the present invention comprises the following steps:
(1) prepare ginkgolides enriched substance: get ginkgo biloba p.e (EGB), organic solvent extractingGet, extract evaporated under reduced pressure, obtains ginkgolides enriched substance;
(2) anti-phase polymeric adsorbent column chromatography: ginkgolides enriched substance is passed through anti-phase polymeric adsorbent,First use the ethanol elution 1-4BV removal of impurities of 0-20%, then use 20%-50% ethanol elution resin 1-8BV,Collect containing the eluent of Bilobalide and reclaim solvent to dry, obtain Bilobalide crude product;
(3) recrystallization: after Bilobalide crude product filters by 10%-60% ethanol heating for dissolving, 2 DEG C12-48h is placed in-10 DEG C of refrigerations, crystallization, and repeated crystallization 1-3 time, brilliant with purifying washing1-5 time, in 60 DEG C of-120 DEG C of vacuum dryings, obtain high-purity Bilobalide.
Described BV is art-recognized wash-out column volume unit.
The isolation and purification method of Bilobalide of the present invention, described step (1) ginkgo biloba p.e(EGB) be commercially available, or prepare by following method: taking ginkgo cured leaf as raw material, pulverize, use40%-80% ethanol water extracts, and extracting solvent load is 4-8 times of W/V of medicinal material amount, extractsNumber of times is 3-4 time, and each extraction time is 1-2 hour, merges extract, and reduced pressure concentration returnsReceive ethanol to without after ethanol taste, filter, macroporous absorbent resin D101 or HP20 post on filtrate,Column volume is that the 1-1.5 of medicinal material amount doubly measures W/V, washing 2-3BV impurity elimination, and 60%-80% ethanol is washedTake off thin out to eluent color till, reduced pressure concentration eluent obtains ginkgo biloba p.e.
The organic solvent of step (1) is selected from ethyl acetate, methyl acetate, propyl acetate, acetic acidOne or both mixed solvents in butyl ester, acetone, methyl ethyl ketone, n-butanol or isobutanolExtraction, ethyl acetate or acetone, extraction times is 1-6 time, preferably 3 times, extraction at every turnGetting solvent for use consumption is that ginkgo biloba p.e 5-15 doubly measures W/V, preferably 10 times of amount W/V.
Described step (2) by anti-phase polymeric adsorbent column chromatography gained containing Bilobalide stream part in55 DEG C-65 DEG C and-0.09--0.1MPa condition under vacuum rotary steam do to solvent-free, 40 DEG C-70 DEG CHeating for dissolving, in 10%-60% ethanol, is filtered while hot, and filtrate is placed under 2 DEG C of-10 DEG C of conditions12-48 hour, crystallization, filters and obtains Bilobalide crude product.
The described anti-phase polymeric adsorbent filler of step (2) is the anti-phase absorption tree of MCI-GELCHP seriesFat or the anti-phase polymeric adsorbent of NM100 series.
The anti-phase polymeric adsorbent of described MCI-GELCHP series is that Mitsubishi chemical Co., Ltd produces,Model is CHP20/P120, and its technical parameter is: particle diameter is 75-150 μ m, and average grain diameter is120 μ m, PH scope is 0-14, and aperture is 450 dusts, and matrix is polystyrene and divinylCopolymer.
The anti-phase polymeric adsorbent of described NM100 series is that Suzhou Nano-micro Technology Co., Ltd. produces, typeNumber be NM100, its technical parameter is: particle diameter is 50-150 μ m, and aperture is 300 dusts, matrixFor polystyrene and divinylbenzene.
Removal of impurities solvent is 0-20% ethanolic solution, preferably 10% ethanolic solution, and elution volume is1-4BV, preferably 1-2BV;
Eluting solvent is 20-50% ethanol, preferably 30-40% ethanol, and elution volume is 3-10BV,Preferably 6-8BV.
Described step (3) recrystallisation solvent is 10%-60% ethanol; Re-crystallization step is for repeatedly heavily tyingBrilliant 1-3 time; Wash crystallisation step for washing crystallization 1-5 time with purifying.
Preferably recrystallisation solvent is 20%-50% ethanol; Re-crystallization step is for being repeatedly recrystallized 2 times;Wash crystallisation step for washing crystallization 3 times with purifying.
The Bilobalide that the inventive method makes is 98%-99% by detection level.
The inventive method compared with prior art, has obtained good effect:
The filler that the inventive method is used is MCI-GEL or the anti-phase polymeric adsorbent of NM100, shouldFiller has well selective to ginkgolides, can greatly improve the separative efficiency of Bilobalide,And filler can regeneration, the organic solvent poison more used than the column chromatography such as silica gel, aluminium oxideProperty is low, use cost is low.
In addition, the present invention is because the solvent of separation and purification Bilobalide is simple and easy to get, device thereforFor conventional equipment, therefore simple to operate, less energy consumption, adopts nontoxic adsorbent absorption, ethanol solutionInhale, therefore production safety is pollution-free, and products obtained therefrom purity is high, is suitable for suitability for industrialized production,There is larger using value.
Detailed description of the invention
Below by embodiment, the present invention will be further described, instead of in order to limit the present inventionScope.
Embodiment 1
Getting ginkgo biloba p.e (EGB) (commercially available, Total Terpene Lactones content >=6%) 4g is suspended inIn 40mL water, be extracted with ethyl acetate three times, each 50mL, extraction solution in 60 DEG C and-0.09-Decompression and solvent recovery under-0.1MPa condition, extract is ginkgolides enriched substance, HPLC-ELSDDetecting total ginkgolides content is 34.5%, and extract 60oC heating is dissolved in 100mL water, usesThe MCI-GEL resin of 100mL adsorbs, and adsorption time is 0.5h, first uses 10% ethanolWash-out 3BV removal of impurities, then use 30% ethanol elution resin 8BV, after detecting, collects containing gingko HPLCLactone eluent, in 65 DEG C and-0.09--0.1MPa condition under, vacuum rotary steam is done to solvent-freeObtain Bilobalide crude product, Bilobalide crude product adds 40% ethanol (2.8mL), and 60 DEG C add thermosolXie Hou, places refrigerator (4 DEG C) 24h, and crystallization, is recrystallized 2 times repeatedly, uses purified water(each 1mL) washes brilliant 3 times, dries in 65 DEG C of heating in vacuum, obtains Bilobalide 83mg,HPLC-ELSD detection level is 98.4%.
The detection method of ginkgolides and Bilobalide is selected HPLC-ELSD detection method (bibliographyFor medical Leader, in March, 2010,29(3): 377-378).
Embodiment 2
Getting ginkgo biloba p.e (EGB) (commercially available, Total Terpene Lactones content >=6%) 4g is suspended inIn 40mL water, be extracted with ethyl acetate three times, each 50mL, extraction solution reduces pressure in 60oCReclaim solvent, extract is ginkgolides enriched substance, and HPLC-ELSD detects total ginkgolides and containsAmount is 31.8%, and 60 DEG C of heating of extract are dissolved in 100mL water, with the NM100 tree of 100mLFat adsorbs, and adsorption time is 0.5h, first uses 10% ethanol elution 3BV removal of impurities, then uses30% ethanol elution resin 8BV, collects containing Bilobalide eluent, in 65oC after HPLC detectsUnder-0.09--0.1MPa condition, vacuum rotary steam is done to solvent-free Bilobalide crude product, returnsReceive solvent, Bilobalide crude product adds 40% ethanol (2.6mL), after 60 DEG C of heating for dissolving, putsPut refrigerator (4 DEG C) 24h, crystallization, is recrystallized 2 times repeatedly, with purified water (1mL)Wash brilliant 3 times, dry in 65 DEG C of heating in vacuum, obtain Bilobalide 71mg, HPLC-ELSDDetection level is 98.8%.
Embodiment 3
Get dry Folium Ginkgo (commercially available) 300g, pulverize, 80% alcohol reflux extracts three times, and solvent is usedAmount be followed successively by 2.4L, 1.5L and 1.5L, extract 2h at every turn, merge extract, 60 DEG C andUnder-0.09--0.1MPa condition, be evaporated to without ethanol taste, filter, on filtrate, macropore is inhaledAttached resin D101 post, purified water (1000mL) is washed post impurity elimination, and 70% ethanol (2000mL) is washedTake off to eluent color thin out (thin-layer chromatography detects without ginkgo biloba p.e), eluent in60 DEG C and-0.09--0.1MPa condition under, vacuum rotary steam is done to solvent-free ginkgo biloba p.e(6g), HPLC-ELSD detection Total Terpene Lactones content is 6.5%
Ginkgo biloba p.e 6g is extracted with ethyl acetate three times, each 150mL, extraction solution in60 DEG C of evaporated under reduced pressure reclaim solvent, and extract is ginkgolides enriched substance, and HPLC-ELSD detectsTotal ginkgolides content is 29.3%, and 60 DEG C of heating for dissolving of extract, in 20mL water, are used 70mLMCI-GEL resin adsorb, adsorption time is 1h, first removes with 10% ethanol elution 3BVAssorted, then use 30% ethanol elution resin 6BV, after detecting, collects containing Bilobalide eluent HPLC,In 65 DEG C and-0.09--0.1MPa condition under, vacuum rotary steam is done to solvent-free reduced pressure concentration dryBilobalide crude product, reclaims solvent, and Bilobalide adds 30% ethanol 3.8mL, and 60 DEG C add thermosolXie Hou, places refrigerator (4 DEG C) 24h, and crystallization, is recrystallized 3 times repeatedly, uses purified water(1.5mL) wash brilliant 3 times, dry in 80 DEG C of heating in vacuum, obtain Bilobalide 102mg,HPLC-ELSD detection level is 98.5%.
Embodiment 4
Get dry Folium Ginkgo (commercially available) 500g, pulverize, 80% alcohol reflux extracts three times, and solvent is usedAmount be followed successively by 4L, 2.5L and 2.5L, extract 2h at every turn, merge extract, 60 DEG C and-0.09-Under-0.1MPa condition, be evaporated to without ethanol taste, filter macroporous absorbent resin on filtrateD101 post, purified water (1500mL) is washed post impurity elimination, and 70% ethanol (3000mL) is eluted toDe-liquid color thin out (thin-layer chromatography detects without ginkgo biloba p.e), eluent is in 60 DEG CUnder-0.09--0.1MPa condition, the dry ginkgo biloba p.e (7.2g) that to obtain of reduced pressure concentration,It is 9.9% that HPLC-ELSD detects Total Terpene Lactones content.
Ginkgo biloba p.e 7.2g is extracted with ethyl acetate three times, each 250mL, extraction solutionReclaim solvent in 60oC evaporated under reduced pressure, extract is ginkgolides enriched substance, HPLC-ELSD inspectionSurveying total ginkgolides content is 31.8%, and 60 DEG C of heating for dissolving of extract, in 40mL water, are usedThe NM100 resin of 100mL adsorbs, and adsorption time is 1h, first uses 10% ethanol elution 3BVRemoval of impurities, then use 30% ethanol elution resin 6BV, after detecting, collects containing Bilobalide wash-out HPLCLiquid, in 65 DEG C and-0.09--0.1MPa condition under, vacuum rotary steam is done to solvent-free gingkoEster crude product, reclaims solvent, and Bilobalide adds 50% ethanol 4.2mL, after 60 DEG C of heating for dissolving,Place refrigerator (4 DEG C) 24h, crystallization, is recrystallized 3 times repeatedly, with purified water (1.5mL)Wash brilliant 3 times, dry in 80 DEG C of heating in vacuum, obtain Bilobalide (153mg, HPLC-ELSDDetection level is 98.4%).
Embodiment 5
Prepare ginkgolides enriched substance (1.8g) by the method for embodiment 3, HPLC-ELSD detectsTotal ginkgolides content is 37.6%, and extract 60oC heating for dissolving, in 20mL water, is used 70mLMCI-GEL resin adsorb, adsorption time is 1.5h, first uses 10% ethanol elution 4BVRemoval of impurities, then use 25% ethanol elution resin 8BV, after detecting, collects containing Bilobalide wash-out HPLCLiquid, in 60 DEG C and-0.09--0.1MPa condition under, vacuum rotary steam is done to solvent-free reduced pressure concentrationDo to obtain Bilobalide crude product, reclaim solvent, Bilobalide adds 25% ethanol 6.8mL, and 50 DEG C addAfter heat of solution, place refrigerator (4 DEG C) 36h, crystallization, is recrystallized 2 times, repeatedly with pureChange water (1.5mL) and wash brilliant 3 times, dry in 60 DEG C of heating in vacuum, obtain Bilobalide 205mg,HPLC-ELSD detection level is 98.7%.
Embodiment 6
Prepare ginkgolides enriched substance (3.3g) by the method for embodiment 4, HPLC-ELSD detectsTotal ginkgolides content is 18.6%, and extract 60oC heating for dissolving, in 40mL water, is used 100mLNM100 resin adsorb, adsorption time is 1.5h, first removes with 10% ethanol elution 3BVAssorted, then use 35% ethanol elution resin 6BV, after detecting, collects containing Bilobalide eluent HPLC,In 55 DEG C and-0.09--0.1MPa condition under, vacuum rotary steam is done to solvent-free Bilobalide thickProduct, reclaim solvent, and Bilobalide adds 45% ethanol 6.2mL, after 60 DEG C of heating for dissolving, placeRefrigerator (4 DEG C) 24h, crystallization, is recrystallized 3 times repeatedly, washes by purified water (1.5mL)Brilliant 3 times, dry in 70 DEG C of heating in vacuum, obtain Bilobalide (241mg, HPLC-ELSDDetection level is 98.8%).
Claims (10)
1. an isolation and purification method for Bilobalide, is characterized in that, the method comprises followingStep:
(1) prepare ginkgolides enriched substance: get ginkgo biloba p.e, ethyl acetate extraction, subtractsPress evaporate to dryness to obtain ginkgolides enriched substance;
(2) anti-phase polymeric adsorbent column chromatography: ginkgolides enriched substance by MCI-GELCHP isBe listed as anti-phase polymeric adsorbent or the anti-phase polymeric adsorbent of NM100 series, first use the ethanol elution of 0-20%1-4BV removal of impurities, then use 20%-50% ethanol elution resin 1-8BV, collect washing containing BilobalideDe-liquid reclaims solvent to dry, obtains Bilobalide crude product;
(3) recrystallization: after Bilobalide crude product filters by 10%-60% ethanol heating for dissolving, 2 DEG C12-48h is placed in-10 DEG C of refrigerations, crystallization, and repeated crystallization 1-3 time, brilliant with purifying washing1-5 time, in 60 DEG C of-120 DEG C of vacuum dryings, obtain high-purity Bilobalide; In described gingkoEster content is 98%-99%.
2. the isolation and purification method of a kind of Bilobalide according to claim 1, its featureBe, described step (1) ginkgo biloba p.e is commercially available, or prepares by following method: withGinkgo cured leaf is raw material, pulverizes, and with the extraction of 40%-80% ethanol water, extracts solvent loadFor 4-8 times of W/V of medicinal material amount, extraction time is 3-4 time, and each extraction time is that 1-2 is littleTime, merging extract, reduced pressure concentration reclaims ethanol to without after ethanol taste, filters, large on filtrateMacroporous adsorbent resin D101 or HP20 post, column volume is that the 1-1.5 of medicinal material amount doubly measures W/V, washing2-3BV impurity elimination, till 60%-80% ethanol elution is thin out to eluent color, reduced pressure concentration wash-outLiquid obtain ginkgo biloba p.e.
3. the isolation and purification method of a kind of Bilobalide according to claim 1, its featureBe, described step (1) ethyl acetate extraction times is 1-6 time, extracts solvent for use at every turnConsumption is that ginkgo biloba p.e 5-15 doubly measures W/V.
4. the isolation and purification method of a kind of Bilobalide according to claim 3, is characterized in that,Described step (1) ethyl acetate extraction times is 3 times, extracts solvent for use consumption for silver at every turn10 times of amount W/V of apricot leaf extract.
5. the isolation and purification method of a kind of Bilobalide according to claim 1, is characterized in that,The anti-phase polymeric adsorbent of described step (2) MCI-GELCHP series is that Mitsubishi chemical Co., Ltd is rawProduce, model is CHP20/P120, and its technical parameter is: particle diameter is 75-150 μ m, average particleFootpath is 120 μ m, and PH scope is 0-14, and aperture is 450 dusts, and matrix is polystyrene and twoEthylenic copolymer; The anti-phase polymeric adsorbent of described NM100 series is that the limited public affairs of micro-science and technology are received in SuzhouDepartment produces, and model is NM100, and its technical parameter is: particle diameter is 50-150 μ m, and aperture is300 dusts, matrix is polystyrene and divinylbenzene.
6. the isolation and purification method of a kind of Bilobalide according to claim 1, is characterized in that,Described step (2) removal of impurities solvent is 0-20% ethanolic solution, and elution volume is 1-4BV; Wash-outSolvent is 20%-50% ethanol, and elution volume is 3-10BV.
7. the isolation and purification method of a kind of Bilobalide according to claim 6, is characterized in that,Described step (2) removal of impurities solvent is 10% ethanolic solution, and elution volume is 1-2BV; Wash-out is moltenAgent is 30%-40% ethanol, and elution volume is 6-8BV.
8. the isolation and purification method of a kind of Bilobalide according to claim 1, is characterized in that,Described step (2) is by the MCI-GELCHP anti-phase polymeric adsorbent of series or the anti-phase suction of NM100 seriesAttached resin column chromatography gained containing Bilobalide stream part in 55 DEG C-65 DEG C and-0.09--0.1MPa barUnder part, vacuum rotary steam is done to solvent-free, 40 DEG C of-70 DEG C of heating for dissolving in 10%-60% ethanol,Filter while hot, filtrate is placed 12-48 hour under 2 DEG C of-10 DEG C of conditions, and crystallization filtersObtain Bilobalide crude product.
9. a kind of isolation and purification method of Bilobalide according to claim 1, is characterized in that,The solvent of described step (3) crystallization is 10%-60% ethanol; Recrystallization is the 1-3 that is repeatedly recrystallizedInferior; With purifying washing crystallization 1-5 time.
10. a kind of isolation and purification method of Bilobalide according to claim 9, is characterized in that,Described step (3) recrystallisation solvent is 20%-50% ethanol; Recrystallization is for being repeatedly recrystallized 2 times;With purifying washing crystallization 3 times.
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| US6590109B2 (en) * | 2001-07-11 | 2003-07-08 | The Trustees Of Columbia University In The City Of New York | Method for isolating terpene trilactones (ginkgolides, bilobalide) from leaves and pharmaceutical powders of ginkgo biloba |
| CN101134758A (en) * | 2007-10-15 | 2008-03-05 | 桂林市振达生物科技有限责任公司 | Method for extracting and separating bilobalide A, B, C, J and bilobalide monomer from ginkgo leaf |
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| US6590109B2 (en) * | 2001-07-11 | 2003-07-08 | The Trustees Of Columbia University In The City Of New York | Method for isolating terpene trilactones (ginkgolides, bilobalide) from leaves and pharmaceutical powders of ginkgo biloba |
| CN101134758A (en) * | 2007-10-15 | 2008-03-05 | 桂林市振达生物科技有限责任公司 | Method for extracting and separating bilobalide A, B, C, J and bilobalide monomer from ginkgo leaf |
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