CN1379029A - Process for extracting ginkgolectone AB - Google Patents

Abstract

A process for extracting ginkgolectone AB includes such steps as immersion extracting, purifying by column, extracting, separation and crystallization. Its advantages are high extracting rate (about 0.2% extracting from leaf) and quality, and high purity (more than 95%).

Description

Process for extracting ginkgolectone AB

The present invention relates to a kind of technology of from Ginkgo Leaf, extracting bilobalide.

Folium Ginkgo terpene lactones is to coexist as biologically active substance in the Ginkgo Leaf with ginkgolic flavone glycoside, and bilobalide is mainly the anti-platelet aggregation factor, and bilobalide is neural, psychosis medicine, and senile dementia is had unusual curative effect.Along with going deep into of research, pharmacological evaluation and clinical confirmation, each component and biological activity more and more cause people's attention in the Folium Ginkgo terpene lactones.Therefore, people are also more and more deep to the research of extracting the Folium Ginkgo terpene lactones method.But mostly present extracting method both domestic and external is to adopt the separation of terpene lactones mixture, and the problem of this method is a unstable product quality, and purity is low, and extraction yield is low.

The objective of the invention is to: provide a kind of and separate Folium Ginkgo terpene lactones AB, quality product and output all are improved, and production cost is low, be fit to suitability for industrialized production with chromatography.

The present invention is achieved in that it comprises lixiviate, column purification, extraction, separation, several steps of crystallization:

(1) get Ginkgo Leaf and add vat liquor, be heated to 30～80 ℃, 30 minutes～2 hours after-filtration of lixiviate, residue add vat liquor 30～80 ℃ of following lixiviates 30 minutes～2 hours, refilter, and merge vat liquor, reclaim solvent;

(2) concentrated solution adds and is water-cooled to below 60 ℃, staticly settles 8 hours, crosses adsorption column, and effluent liquid carries out saturated check, goes up sample as saturated then stopping, and water is crossed post, crosses post with alcohol again, collects effluent liquid, recovered alcohol, vacuum-drying, crude extract;

(3) with the crude extract dissolution with solvents, peroxidation aluminium post is collected effluent liquid, treats that post need change post after saturated again;

(4) be 30% with effluent liquid vacuum concentration to the dry rate of collecting, the crystal of separating out is Ginkgolide A and Ginkgolide B, and ginkalide C and bilobalide are stayed in the mother liquor, use the suction filter isolation of crystalline, and gets ginkgolectone AB with ethyl alcohol recrystallization.

The present invention compared with prior art, it is reasonable to have an operational path, extraction yield height, advantages such as good product quality.Its purity can reach more than 95%, and total yield is in (leaf extraction) and about 3% (GBE extraction) about 0.2%.

Embodiments of the invention:

(1) gets 10kg DA201 resin, soaked 48 hours, under the tap water flushing of crossing microporous membrane, filter out 20～60 orders with sub-sieve, 60～80 purpose resins, get 20～60 order resin 2000g, after cleaning up repeatedly with distilled water, add 2mol/L NaOH 10L, soaked 4 hours, be washed till nearly neutrality with distilled water, add 4mol/L HCl 10L, soaked 8 hours, be washed till nearly neutrality with distilled water, the ethanol 10L of adding 80% soaked 10 hours, cleaned repeatedly to alcohol-free flavor with distilled water, stand-by with distilled water immersion, the dress post in the resin of packing into, can not have bubble in the middle of the resin;

(2) get Ginkgo Leaf 1000g and add 60% alcohol 9000ml, in water-bath internal heating to 60～70 ℃, lixiviate 2 hours was stirred once, and was used filtered through gauze in per 10 minutes, residue adds 60% alcohol 7000ml, 60～70 ℃ of following lixiviates 2 hours, stirred once, and refiltered in per 10 minutes, merge vat liquor, with film under vacuum vaporizer recovered alcohol;

(3) concentrated solution adds water to about 4000ml, be cooled to below 60 ℃, staticly settled 8 hours, cross the DA201 resin column, cross column flow rate and be controlled at 0.5ml/s, every 2 minutes effluent liquid is carried out saturated check, go up sample, cross post with distilled water as saturated then stopping, to effluent liquid limpid till, cross post with 80% alcohol 2000ml again, collect the darker effluent liquid of color, film under vacuum vaporizer recovered alcohol, the vacuum drying oven drying, vacuum tightness is-0.07～0.08MPa, and temperature is 70 ℃, gets crude extract (GBE);

(4) with crude extract 1000ml 95% dissolve with ethanol, the peracidity alumina column is collected effluent liquid, treats that post need change post after saturated again;

(5) be 30% with effluent liquid vacuum concentration to the dry rate of collecting, have a large amount of crystal to separate out this moment, the crystalline body composition is Ginkgolide A and Ginkgolide B, and ginkalide C and bilobalide are stayed in the mother liquor, uses the suction filter isolation of crystalline, and wash crystal with a small amount of 95% ethanol, with crystal once, get ginkgolectone AB, purity＞90% with 95% ethyl alcohol recrystallization, again recrystallization once, ginkgolectone AB purity＞95%.

Cross post with 80% alcohol 1000ml, cross post with 2000ml water again, effluent liquid is discarded, and purification column is promptly reusable.

Claims (1)

1, a kind of process for extracting ginkgolectone AB, it comprises lixiviate, column purification, extraction, separation, several steps of crystallization, it is characterized in that:

(1) get Ginkgo Leaf and add vat liquor, be heated to 30～80 ℃, 30 minutes～2 hours after-filtration of lixiviate, residue add vat liquor 30～80 ℃ of following lixiviates 30 minutes～2 hours, refilter, and merge vat liquor, reclaim solvent;

(2) concentrated solution adds and is water-cooled to below 60 ℃, staticly settles 8 hours, crosses adsorption column, and effluent liquid carries out saturated check, goes up sample as saturated then stopping, and water is crossed post, crosses post with alcohol again, collects effluent liquid, recovered alcohol, vacuum-drying, crude extract;

(3) with the crude extract dissolution with solvents, peroxidation aluminium post is collected effluent liquid, treats that post need change post after saturated again;

(4) be 30% with effluent liquid vacuum concentration to the dry rate of collecting, the crystal of separating out is Ginkgolide A and Ginkgolide B, and ginkalide C and bilobalide are stayed in the mother liquor, use the suction filter isolation of crystalline, and gets ginkgolectone AB with ethyl alcohol recrystallization.