Method for simultaneous preparing high-purity total flavonol glycosides and ginkgolides

Abstract

A method for simultaneous separating total flavonol glycosides and ginkgolides from ginkgo biloba extract is provided. The method is characterized in that the ginkgo biloba extract is taken as a raw material, column chromatography enrichment and purification through polyamide and macroporous resin are conducted, after eluent is concentrated, ester solution is added for extraction, an organic phase part is washed with water, standing is conducted for stratification, an aqueous phase and an organic phase are combined correspondingly, an solvent is recovered, drying and smashing are conducted, and then the high-purity total flavonol glycosides and the ginkgolides are obtained. According to the method for simultaneous separating the total flavonol glycosides and the ginkgolides from the ginkgo biloba extract, it is guaranteed that the purity of the total flavonol glycosides simultaneously separated from the ginkgo biloba extract reaches 90% or more, the transfer rate is not less than 65%, the purity of the total of the sum of ginkgolides A, ginkgolides B and ginkgolides C is more than 85% or more, the transfer rate of the sum of the ginkgolides is not less than 55%, and total ginkgolic acid contained is less than 1mg / kg; organic extraction is combined with water washing so that the high-purity total flavonol glycosides and the ginkgolides can be simultaneously obtained with rapid speed and low cost, residue organic solvents is low, and sensitization substance is less or few.

Description

technical field [0001] The invention belongs to the field of medicine, and in particular relates to a method for simultaneously preparing total flavonol glycosides and ginkgolides. Background technique [0002] One of the main active ingredients of Ginkgo biloba extract is flavonoids, including quercetin, kaempferol, isorhamnetin and flavonol glycosides, etc. Flavonol glycosides exist in the form of flavonoids, which can expand coronary blood vessels and lower serum cholesterol. Ginkgolides are another class of active ingredients in Ginkgo biloba extract, including ginkgolide A (C 20 h 24 o 9 ), ginkgolide B (C 20 h 24 o 10 ), ginkgolide C (C 20 h 24 o 11 ), etc., have the effect of inhibiting platelet aggregation and neuroprotection. These two types of ingredients are the active ingredients in the ginkgo biloba extract preparation represented by Shuxuening injection. [0003] At present, the production techniques of total flavonol glycosides of Ginkgo biloba main...

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Problems solved by technology

Publication numbers CN1335157A, CN103372034A, and CN102416027A use ginkgo leaves as starting materials to prepare total flavonoids and ginkgolides respectively through extraction, polyamide column (or macroporous resin column), extraction and other steps, but the purity of total flavonol glycosides is low. Low, only about 50%; CN102552340A provides a preparation method for the preparation of ginkgo terpenoid monomers and ginkgo total flavonoids, the method uses ginkgo standard extract EGB761 as raw material, after dissolution, purified by polyamide resin, refrigerated, precipitated , extraction, recrystallization and other steps to prepare ginkgolides (precipitation and recrystallization steps take 1-10 days and 1-2 days respectively), and then prepare total flavonoids by using anion exchange resin and machine composite membrane nanofiltration equipment, etc., the whole The production cycle of the process is long and requires high equipment, which is not suitable for industrial production; CN1508542A mentions a method for simultaneously preparing ginkgolides and total flavonoids, wherein the preparation of ginkgolides needs to be extracted, recrystallized, activated carbon and silica gel. Column separation; the preparation of total flavonoids needs to go through the polyamide column twice and the silica gel column once, the process operation is complicated, and the product transfer rate is low; CN102283870A is to put the crude extract of ginkgo on the ADS-F8 resin column, using 10% and 70% respectively % ethanol for elution, collect the eluent respectively to obtain total ginkgo flavonoids and ginkgolides, the total ginkgo flavonoids are subjected to cold and heat treatment to obtain refined ginkgo total flavonoids, and ginkgolides are extracted with ethyl acetate to obtain ginkgolide refined substances, But the yield is low (less than 1%); CN1847237A uses Ginkgo biloba as raw material, and prepares ginkgolides and total flavonoids respectively through extraction, crossing the macroporous resin column and intercepting different eluents, but the purity of both is not enough, about 80% About this patent, the method for further refining ginkgolides is also given, involving activated carbon adsorption, centrifugal impurity removal, microfiltration membrane fine filtration, etc., the operation is complicated, and the product transfer rate is low; The resin column enriches the total flavonol glycosides and total lactones, and then extracts them with ethyl acetate aqueous solution, the aqueous phase passes through the glucose gel to prepare the total flavonol glycosides, and the ethyl acetate phase is directly concentrated to obtain ginkgolides. The process steps of this method Simple, but its product transfer rate is still not ideal and needs to be further improved