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Method for preparing quercetin-3-o-glucoside from ginkgo leaf extract

A technology of glucoside and extract, which is applied in the field of compound preparation, can solve problems such as less strict and standardized effects, different drug effects, and restrictions on drug quality standards, and achieve improved drug quality standards, simple preparation methods, and convenient separation operations Effect

Active Publication Date: 2017-01-04
北京华润高科天然药物有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, Ginkgo biloba extract is a very complex compound-enriched product, containing various components ranging from inorganic to organic, from polar to non-polar, from small molecules to biomacromolecules. According to incomplete statistics, Ginkgo biloba contains 240 There are multiple chemical components, but there are only a dozen peaks in the fingerprint of ordinary ginkgo biloba extract, which cannot accurately and accurately reflect the material basis of the product
It is well known that the extraction methods of ginkgo leaf extract are different, the effective compounds and their contents in the obtained extracts are different, and the medicinal effects are also different, and the applicable symptoms and functions of the medicines prepared from them must not be completely the same; Strictly speaking, even if the extraction method is the same, due to the different batches of ginkgo biloba raw materials and different products, the content of chemical components in the final extract is not the same, and the above factors will eventually have different degrees of influence on the efficacy of the drug. Therefore, the quality control of Ginkgo biloba extract and its preparations is not very strict and standardized only with the current quality standards. The existence of a large number of unknown substances affects the accurate determination of its content and restricts the improvement of drug quality standards.

Method used

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  • Method for preparing quercetin-3-o-glucoside from ginkgo leaf extract
  • Method for preparing quercetin-3-o-glucoside from ginkgo leaf extract
  • Method for preparing quercetin-3-o-glucoside from ginkgo leaf extract

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Experimental program
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Effect test

Embodiment 1

[0027] Weigh 10 g of Ginkgo biloba extract, dissolve it in 50 mL of 40% ethanol-water solution to obtain a Ginkgo biloba extract solution with a concentration of 200 mg / mL, pass it through a 0.45 μm microporous membrane, and perform one-dimensional liquid chromatography separation. One-dimensional liquid chromatography adopts silica gel as the matrix of hydrophilic chromatographic filler 50 × 250mm, 10 μm (Huapu New Innovation Technology Co., Ltd.), and the mobile phase adopts methanol containing 0.1% volume concentration of formic acid as the organic phase, containing 0.1% volume The water with formic acid concentration is the water phase, and the gradient elution method: the concentration of the organic phase decreases from 95% to 90% in step gradient in 0-15min. Use DAD ultraviolet detector 360nm to select the absorption wavelength, the preparation temperature is room temperature, the injection volume is 500μL / needle, the mobile phase flow rate is 90mL / min, the fractions col...

Embodiment 2

[0035] Weigh 1 g of Ginkgo biloba extract, dissolve it in 100 mL of ethanol-water solution with a volume concentration of 80%, and obtain a Ginkgo biloba extract solution with a concentration of 10 mg / mL, pass it through a 0.45 μm microporous membrane, and perform one-dimensional liquid chromatography. One-dimensional liquid chromatography adopts silica gel-based hydrophilic chromatographic packing (50×250mm, 10μm, Huapu Innovation Technology Co., Ltd.), the mobile phase uses ethanol as the organic phase, water as the aqueous phase, and the concentration of the organic phase is 90 % isocratic, using a DAD ultraviolet detector at 360nm to select the absorption wavelength, the preparation temperature is 40°C, the injection volume is 200μL / needle, the flow rate of the mobile phase is 60mL / min, the fractions collected for 15-20 minutes are concentrated to dryness by rotary evaporation , for the one-dimensional preparation of crude quercetin-3-O-glucoside. Dissolve the crude querce...

Embodiment 3

[0038] Weigh 100g of Ginkgo biloba extract, dissolve it in 200mL of 50% ethanol-water solution to obtain a Ginkgo biloba extract solution with a concentration of 500mg / mL, pass it through a 0.45μm microporous membrane, and prepare it by one-dimensional liquid chromatography. One-dimensional liquid chromatography adopts a hydrophilic chromatographic packing (50×250mm, 10 μ, Huapu Innovation Technology Co., Ltd.) based on silica gel, and the mobile phase adopts ethanol (containing 0.1% formic acid) as the organic phase, water (containing 0.1% % formic acid) is the aqueous phase, and is eluted by 95% organic equivalence. The DAD ultraviolet detector is used to select the absorption wavelength at 360nm, the preparation temperature is 30°C, the injection volume is 3000μL / needle, the flow rate of the mobile phase is 120mL / min, the fractions collected for 15-20 minutes are concentrated to dryness by rotary evaporation, and the one-dimensional Prepare crude quercetin-3-O-glucoside. D...

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Abstract

The invention discloses a method for preparing quercetin-3-o-glucoside from ginkgo leaf extract. The method for preparing quercetin-3-o-glucoside from ginkgo leaf extract comprises the following steps of dissolving ginkgo leaf extract in ethanol-water solution to prepare ginkgo leaf extract solution; performing one-dimensional liquid chromatographic separation on the extract solution to obtain one-dimensional crude products; dissolving the one-dimensional crude products into methanol-water solution or ethanol-water solution to obtain crude product solution; performing two-dimensional liquid chromatographic separation on the crude product solution to obtain quercetin-3-o-glucoside. The invention prepares a definite medicinal compound, i.e., quercetin-3-o-glucoside from ginkgo leaf extract, the method for preparation is simple, the separation operation is convenient to perform, a specific compound is separated by adopting two-dimensional liquid chromatography, thus an index component is added in studies on quality control of ginkgo leaf extract, detection objects of active substances are enriched, and the improvement of ginkgo leaf extract and medicine quality standards thereof is facilitated.

Description

technical field [0001] The invention relates to an extraction and preparation method of an active ingredient in ginkgo leaf extract, in particular to a method for preparing quercetin-3-o-glucoside from ginkgo leaf extract, which belongs to the technical field of compound preparation. Background technique [0002] Ginkgo biloba is the dried leaf of Ginkgo biloba plant, Ginkgo biloba extract is the enriched product of active substances extracted from Ginkgo biloba through modern extraction technology, which can be used for Alzheimer's disease, depression, diabetes, neurological diseases, impotence , memory impairment, peripheral vascular disease, intermittent claudication, brain turning tinnitus and other diseases. Its main active ingredients are flavonoids and terpenes. Flavonoids include monoflavones, flavonol glycosides, acetylated flavonol glycosides, biflavones, flavan-3-ols, and proanthocyanidins. Terpenoid ginkgolides include ginkgolides A, B, C, J, M and bilobalide. ...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08
Inventor 王秋平丰加涛陈利敏
Owner 北京华润高科天然药物有限公司
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