Method for preparing kaempferol-3-O-2'',6''-dirhamnosylglucoside

A technology of -3-O-2 and rhamnosyl, which is applied in the field of medicine, can solve the problems of large organic solvent consumption, cumbersome operation steps, time-consuming and labor-intensive, etc., and achieve a high degree of instrument automation, abundant resources, and convenient operation Effect

Active Publication Date: 2013-05-22
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

At present, the extraction and separation of kaempferol-3--2”, 6”-dirhamnosyl glucoside is mainly carried out through alcohol extraction of plants, and then multiple column chromatography steps such as macroporous resin or dextran gel. Separation and purification, the operation steps are cumbersome, the process is complicated, and it needs to consume a large amount of organic solvents, which is time-consuming and laborious
The method of preparing kaempferol-3-O-2",6"-dirhamnosyl glucoside by two-dimensional liquid chromatography-mass spectrometry has not been reported yet

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Weigh 500g of Ginkgo biloba extract, dissolve it in 1L of 50% methanol-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. The one-dimensional liquid chromatography adopts XUnion C18, the mobile phase adopts acetonitrile as the organic phase, water as the aqueous phase, and the gradient elution method: the concentration of the organic phase increases from 10% to 25% in 20 minutes. Adopt 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 collected for 9-12 minutes are concentrated to dryness by rotary evaporation, which is one-dimensional preparation Kaempferol-3-O-2",6"-dirhamnosyl glucoside crude product. Dissolve the crude kaempferol-3-O-2”, 6”-dirhamnosyl glucoside in 40...

Embodiment 2

[0043] Weigh 2000g of Ginkgo biloba extract, dissolve it in 2L of 25% methanol-water solution to obtain a Ginkgo biloba extract solution with a concentration of 1000mg / mL, pass it through a 0.45μm microporous membrane, and perform one-dimensional liquid chromatography. The one-dimensional liquid chromatography adopts XUnion C8, the mobile phase adopts methanol as the organic phase, water as the aqueous phase, the concentration of the organic phase is 65% isocratic, the absorption wavelength is selected by DAD ultraviolet detector at 360nm, the preparation temperature is 40°C, and the injection volume 200μL / needle, mobile phase flow rate 60mL / min, collect fractions for 5-7 minutes, and concentrate to dryness by rotary evaporation to prepare kaempferol-3-O-2”, 6”-dirhamnosyl for one-dimensional Crude glucoside. Dissolve the crude kaempferol-3-O-2”, 6”-dirhamnosyl glucoside in 50% methanol-water solution to a concentration of 20 mg / mL, filter through a microporous membrane, and p...

Embodiment 3

[0045] Weigh 100g of Ginkgo biloba extract, dissolve it in 10L of 75% methanol-water solution to obtain a Ginkgo biloba extract solution with a concentration of 10mg / mL, pass it through a 0.45μm microporous membrane, and prepare it by one-dimensional liquid chromatography. One-dimensional liquid chromatography adopts Click OEG, the mobile phase adopts methanol containing 0.1% formic acid as the organic phase, and water containing 0.1% formic acid as the aqueous phase, and adopts 5% organic equivalence method for elution. 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, and the fractions collected for 22-25 minutes are concentrated to dryness by rotary evaporation. Preparation of crude kaempferol-3-O-2",6"-dirhamnosyl glucoside. Dissolve the crude kaempferol-3-O-2”, 6”-dirhamnosyl glucoside in 60% methanol-water solution t...

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Abstract

The invention provides a method for preparing kaempferol-3-O-2'',6''-dirhamnosylglucoside, which comprises the following steps: by using a two-dimensional liquid phase chromatography-mass spectroscopy combination technology and taking methanol-water or acetonitrile-water as a mobile phase and a reversed phase C18 chromatographic column as a one-dimensional preparative chromatographic column, performing component cutting on a ginkgo leaf extract, and collecting a target component which is a kaempferol-3-O-2'',6''-dirhamnosylglucoside crude product; and by taking a reversed phase C18 chromatographic column as a two-dimensional preparative chromatographic column, under the guidance of selective ion peaks of mass spectroscopy, performing component cutting on the kaempferol-3-O-2'',6''-dirhamnosylglucoside crude product, collecting, and concentrating through rotary evaporation to obtain the high-purity kaempferol-3-O-2'',6''-dirhamnosylglucoside, wherein the purity can be up to 70% or above. According to the invention, the preparation process is high in repetitiveness and favorable in operability; and meanwhile, ginkgo leaves are abundant in resources and easy to acquire. Thus, the invention meets the requirements for large-scale production and can be used for the preparation of raw materials for a Shuxuening injection.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a method for preparing kaempferol-3-O-2", 6"-dirhamnosyl glucoside. Background technique [0002] Kaempferol-3-O-2", 6"-dirhamnosyl glucoside belongs to flavonoids. Flavonoids have good pharmaceutical effects, can reduce capillary permeability and fragility, promote cell proliferation and prevent Hemagglutination and scavenging of free radicals play a pivotal role in the treatment of cardiovascular and cerebrovascular diseases. At the same time, studies have shown that kaempferol-3-O-2”, 6”-dirhamnosyl glucoside also has anti-tumor effects. [0003] Kaempferol-3-O-2”, 6”-dirhamnosyl glucoside exists in plants such as pearl vegetable, plate bean flower, periwinkle flower, choppie, sea mango, long-leaved succulent, ginkgo biloba and other plants. At present, the extraction and separation of kaempferol-3--2”, 6”-dirhamnosyl glucoside is mainly carried out through alco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08
Inventor 丰加涛付冬梅王海涛冯志琼
Owner 北京华润高科天然药物有限公司
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