CN102293791B - Production method for extracting effective components of gingko leaf - Google Patents
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a production method for extracting effective components of a gingko leaf, which comprises the following steps of: carrying out enzymolysis pretreatment, adding ethanol for reflowing and extracting once; adding glycoside transferase and corresponding saccharide ligand substances and then adding ethanol for reflowing and extracting once; recovering ethanol from the filtered extraction solution and degreasing; carrying out column chromatography and eluting with water and ethanol; and recovering ethanol from an eluent, condensing the eluent in an ointment shape and drying to obtain an extract. The gingko leaf is extracted by using the production method disclosed by the invention, the content of the effective components can be improved by 43-65 percent; and in addition, the production method has the advantages of simpleness in operation, environment friendliness, no toxicity and low production cost.
Description
Technical field
The present invention relates to a kind of production method of extracting effective components in plants, particularly a kind of production method of extracting the effective component of ginkgo leaf that can treat cardiovascular and cerebrovascular disease belongs to the Chinese drug preparation field.
Background technology
Semen Ginkgo is the most ancient in the world Relict Plant, have the title of " living fossil " and " botanic panda ", and China is the native place of Semen Ginkgo, and ginkgo biloba content accounts for more than 70% of world's total amount.The fruit of ginkgo and leaf all have very high medical value and edibility.According to the Compendium of Material Medica record, Semen Ginkgo " prepared food warming the lung and benefiting QI, relieving asthma and cough, urine reducing, only nebulousurine; Eat raw and fall expectorant, sterilization, parasite killing ".Folium Ginkgo extract is widely used in and improves cardio and vascular function at present.Semen Ginkgo is to be familiar with by the foreign study person the earliest and one of the Chinese herbal medicine extensively admitted, and its preparation is best-selling plant amedica in the world.
What in Folium Ginkgo, content was the highest is Flavonoid substances, and terpene lactones is the distinctive baroque compound of Semen Ginkgo, and the effective ingredient such as the flavonoid that extracts from Folium Ginkgo and terpene lactones have positive effect to treatment coronary heart disease, cerebral thrombosis cardiovascular and cerebrovascular disease.At present, the extracting method of ginkgetin compound has the methods such as water extraction, organic solvent extraction, supercritical extraction.The water extraction cost is low, but extracts rate variance, and raw material employing rate is not high; The organic solvent extraction cost is high, and impurity content is high; Though the supercritical fluid method extraction ratio is high, but because of apparatus expensive, universal restricted, the production technology that the CN101708195A patent discloses a kind of Semen Ginkgo extrac on May 19th, 2010, but this technique still exists the effective component of ginkgo leaf extraction ratio not high, the defectives such as not environmental protection, and this technique is extracted, and the content of effective component of ginkgo leaf Flavonoid substances is the highest can only reach 24.5%, therefore, be badly in need of a kind of production method that can effectively improve Flavonoid substances content in Folium Ginkgo.
Summary of the invention
The shortcomings such as the extraction effective component of ginkgo leaf extraction ratio that prior art exists is low in order to overcome, not environmental protection the invention provides and a kind ofly can effectively improve the production method that effective component of ginkgo leaf extracts ratio.
For achieving the above object, the invention provides following technical scheme: a kind of production method of extracting effective component of ginkgo leaf is characterized in that comprising the following steps:
(1) enzymolysis Folium Ginkgo: after the Folium Ginkgo raw material powder was broken into coarse powder, with the enzymolysis solution mix homogeneously, enzymolysis was 1～2 day at the temperature of 30～60 ℃;
(2) extract effective component of ginkgo leaf: the ginkgo powder that enzymolysis is good adds ethanol, reflux, extract, is 1 time at the temperature of 70～85 ℃, add again transglucosidase and corresponding glycosyl ligand substance, then add ethanol, reflux, extract, is 1 time at the temperature of 50-60 ℃, filter, reclaim ethanol, defat after merging the extracting solution of twice; Reclaim ethanol, defat after merging the extracting solution of twice;
(3) upper column chromatography: the extracting solution after defat by macroporous adsorbent resin column chromatography, is then washed with water once successively, with ethanol elution at least three times, after becoming positive section with hydrochloric acid magnesium powder test eluent, merge eluent, reclaim ethanol, be condensed into after paste dry.
After the Folium Ginkgo raw material powder is broken into granule, has increased material with enzymolysis solution and extracted the specific surface area that solvent contacts, raw material fully is dissolved in solvent, can improve extraction ratio.
Temperature has double influence to enzyme, thereby suitable temperature can make enzyme bring into play its maximum activity, also can keep simultaneously its stability preferably, cell wall be carried out cracking, when causing the dissolution with solvents flavone compound to spread to cell surface, resistance reduces, be conducive to the solvent main diffusion, improve the extraction ratio of Ginkgo total flavones, carry out enzymolysis at the temperature of 30～60 ℃, be conducive to make the maximum vigor of enzyme performance when keeping Enzymic stability, make extracting effect reach best; Extraction temperature is directly proportional to lixiviate speed, and temperature raises and can reduce the viscosity of alcohol solvent, thereby improves the extraction efficiency of ginkgetin; But the too high heat stability that might destroy flavone of temperature, the probability of impurity stripping also increases, and can reduce extracting effect on the contrary, therefore keeps suitable temperature just to become very important, and it is best extraction temperature that the present invention is controlled at 70～85 ℃ with temperature.
Further, the enzymolysis solution in described step (1) is the mixture of water and enzyme, and the mass ratio of water and enzyme is 100: 1; The water of enzymolysis solution and the mass ratio of ginkgo leaf powder are 2: 1.
Preferably, described enzyme is the mixture of a kind of and transglucosidase in transglucosidase or cellulase, hemicellulase, pectase, compound enzyme.
Flavone compound in Folium Ginkgo and terpene lactones mainly are wrapped in cell wall take cellulose as main formation, independent ethanol extraction method can't make cell wall break fully, cause the stripping of effective component of ginkgo leaf to have suitable resistance, cause extraction effect to be greatly affected.Folium Ginkgo is carried out the enzyme pretreatment, and enzyme can destroy the cell wall of Folium Ginkgo, make cell wall loose, break, thereby can reduce the stripping resistance of effective component of ginkgo leaf compound, the effective ingredient of Folium Ginkgo is fully dissolved, shorten extraction time, strengthen the extraction effect of effective ingredient.Transglucosidase can make in Folium Ginkgo some ester dissolubility effective ingredient be converted into to improve recovery rate with the hydrophilic composition of glycosyl.At the temperature of 30～60 ℃, Folium Ginkgo is carried out enzymolysis processing, can make the mixture of cellulase or hemicellulase or pectase or compound enzyme and transglucosidase keep good activity, reach the Expected Results of enzymolysis processing.Ginkgo leaf powder after enzymolysis is after the process ethanol extraction, and with respect to the extracting solution that other method obtains, macromolecular substances is relatively less, be convenient to filter, make impurity minimizing in the resin hole, can not stop up the resin hole in chromatography process, make chromatography more abundant, impurity separates more thorough.
Further, described Effect of Alcohol Extracting Procedureto Total was used 30～70% ethanol extraction 2 hours for the first time, used for the second time 30% ethanol extraction 1.5 hours; Ethanol and ginkgo leaf powder mass ratio are 5: 1 for the first time, are 3: 1 for the second time; The mass ratio of the transglucosidase that adds and corresponding glycosyl ligand substance and ginkgo leaf powder is 1～2: 100; Described corresponding glycosyl ligand substance is maltose or glucose.
Extract at the temperature of 70 ℃-85 ℃ with 30～70% ethanol for the first time, purpose is the abundant extraction that is conducive to effective ingredient in Folium Ginkgo, and be convenient to enzyme-added processing for the second time, use for the second time transglucosidase and glycosyl ligand substance that Folium Ginkgo is processed in reflux, extract,, can improve the polarity of flavone aglycone, re-use on this basis 30% ethanol and extract for the second time, further improve the yield of flavonoid glycoside.
Preferably, in described step (2), reflux, extract, adopts multi-function extractor that feed liquid is extracted, and can further increase extraction ratio.
Further, described with ethanol respectively eluting refer to for three times for the first time with 30% ethanol, for the second time with 60% ethanol, for the third time with 80% ethanol eluting respectively.
After extracting solution is crossed post, be eluted to the eluent clarification with purified water, to remove the macromolecular complex in the macroporous resin chromatographic column, removal of contamination, carry out three subgradient eluting with ethanol respectively again, the effective component of ginkgo leaf that is adsorbed on resin column is fully separated with resin column, strengthened the purity of extracting.
Preferably, the macroporous adsorbent resin column chromatography in described step (3) adopts ADX-16 type macroporous adsorptive resins, and this resin is U.S.'s ROHM AND HAAS production, and is strong to ginkgetin and lactone selectivity, can effectively reduce the content of ginkgoic acid.
Beneficial effect of the present invention is as follows:
1, with Folium Ginkgo enzymolysis pretreatment before lixiviate, make the abundant stripping of effective ingredient in Folium Ginkgo, improved greatly lixiviate effect;
2, the present invention adopts extracted many times, uses the method for the ethanol three subgradient eluting of different purity after the pure water eluting again, is conducive to complete stripping and abundant effective ingredient of resolving Folium Ginkgo, and the active constituent content of extraction is improved greatly;
3, enzymolysis pretreatment of the present invention, extracted many times, enzymolysis, chromatography, stepwise elution can improve respectively the extraction ratio of the effective ingredient of Folium Ginkgo, the technical scheme of comprehensive each step, effectively control the technique of stages, can make at last the content of active ingredient in Folium Ginkgo extract improve 43%～65%;
4, simple to operate, the environment-protecting asepsis of production method of the present invention, production cost is low.
The specific embodiment
A kind of production method of extracting effective component of ginkgo leaf of the present invention comprises the following steps:
(1) at first Folium Ginkgo raw material 1000 grams are ground into coarse powder, then 20 gram enzymes are mixed with 2000 gram water, stirring is made into enzymolysis solution, then adds the ginkgo powder of pulverizing, and enzymolysis is 1～2 day at the temperature of 30～60 ℃;
(2) ginkgo leaf powder that above-mentioned enzymolysis is good adds the ethanol (concentration of alcohol that adds in production process can be selected) of 5000 grams 30% between 30～70%, filtering after 2 hours with the multi-function extractor reflux, extract, at the temperature of 70～85 ℃, the maltose that adds again 12ml Suhong475 transglucosidase and 80g/L, filter after 1.5 hours in reflux, extract, at the temperature of 50-60 ℃ with 3000 gram 30% ethanol, reclaim ethanol, defat after collecting the extracting solution of twice;
In production process, the glycosyl ligand substance can also be used glucose; The mass ratio of transglucosidase and corresponding glycosyl ligand substance and ginkgo leaf powder is 1～2: 100, quality raw-material according to Folium Ginkgo in production, corresponding transglucosidase and the glycosyl ligand substance of adding is 1～2: the quality of rational allocation transglucosidase and glycosyl ligand substance in 100 scope;
(3) upper column chromatography: the extracting solution after defat is passed through ADX-16 type macroporous adsorbent resin column chromatography, then wash with water successively once, again with 30% ethanol, 60% ethanol, 80% ethanol difference eluting, after becoming positive section with hydrochloric acid magnesium powder test eluent, merge the eluent of three times, reclaim ethanol, be condensed into after paste dry.
Be below the concrete technology parameter synopsis of each embodiment:
Claims (5)
1. production method of extracting effective component of ginkgo leaf is characterized in that: comprise the following steps:
(1) enzymolysis pretreatment: after the Folium Ginkgo raw material powder was broken into coarse powder, with the enzymolysis solution mix homogeneously, enzymolysis was 1～2 day at the temperature of 30～60 ℃; Described enzymolysis solution is the mixture of water and enzyme, and the mass ratio of water and enzyme is 100:1; The water of described enzymolysis solution and the mass ratio of ginkgo leaf powder are 2:1; Described enzyme is the mixture of a kind of and transglucosidase in transglucosidase or cellulase, hemicellulase, pectase, compound enzyme;
(2) extract effective component of ginkgo leaf: the ginkgo powder that enzymolysis is good adds ethanol, reflux, extract, is 1 time at the temperature of 70～85 ℃, add again transglucosidase and corresponding glycosyl ligand substance, then add ethanol, reflux, extract, is 1 time at the temperature of 50～60 ℃, filter, reclaim ethanol, defat after merging the extracting solution of twice;
(3) upper column chromatography: the extracting solution after defat by macroporous adsorbent resin column chromatography, is then washed with water once successively, with ethanol elution at least three times, after becoming positive section with hydrochloric acid magnesium powder test eluent, merge eluent, reclaim ethanol, be condensed into after paste dry.
2. a kind of production method of extracting effective component of ginkgo leaf according to claim 1, is characterized in that, the Effect of Alcohol Extracting Procedureto Total in described step (2) was used 30～70% ethanol extraction 2 hours for the first time, used for the second time 30% ethanol extraction 1.5 hours; Described ethanol and ginkgo leaf powder mass ratio are 5:1 for the first time, are 3:1 for the second time; The mass ratio of the described transglucosidase that adds and corresponding glucide and ginkgo leaf powder is 1～2:100; Described corresponding glycosyl ligand substance is maltose or glucose.
3. a kind of production method of extracting effective component of ginkgo leaf according to claim 1, is characterized in that, in described step (2), reflux, extract, adopts multi-function extractor that feed liquid is extracted.
4. a kind of production method of extracting effective component of ginkgo leaf according to claim 1, it is characterized in that, in described step (3) with ethanol respectively eluting refer to for three times for the first time with 30% ethanol, for the second time with 60% ethanol, for the third time with 80% ethanol eluting respectively.
5. a kind of production method of extracting effective component of ginkgo leaf according to claim 1, is characterized in that, the macroporous adsorbent resin column chromatography in described step (3) adopts ADX-16 type macroporous adsorptive resins.
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| CN103638071A (en) * | 2013-12-23 | 2014-03-19 | 湖南科技学院 | Efficient production method of gingko medicinal extract |
| CN107661361A (en) * | 2017-11-17 | 2018-02-06 | 浙江工业大学上虞研究院有限公司 | A kind of process for super-critical extracting of ginko leaves flavone class compound |
| CN107669713A (en) * | 2017-11-17 | 2018-02-09 | 浙江工业大学上虞研究院有限公司 | A kind of extraction process of ginko leaves flavone class compound |
| CN108379371A (en) * | 2018-02-06 | 2018-08-10 | 芜湖市诺康生物科技有限公司 | A kind of ginkgo leaf Radix Salviae Miltiorrhizae Fish oil soft capsule and preparation method thereof |
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| CN101032533A (en) * | 2007-04-18 | 2007-09-12 | 黑龙江省珍宝岛制药有限公司 | Method of preparing solution / substance extracted from ginkgo leaves |
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| CN101032533A (en) * | 2007-04-18 | 2007-09-12 | 黑龙江省珍宝岛制药有限公司 | Method of preparing solution / substance extracted from ginkgo leaves |
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| Title |
|---|
| 国内银杏叶化学成分及制备工艺的研究进展;李金生;《白求恩军医学院学报》;20061231;第4卷(第4期);210-222 * |
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