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Separation and purification method of ginkgolide A and B monomer

A technology for separation and purification, ginkgolide, applied in the direction of organic chemistry, bulk chemical production, etc., can solve the problems of methanol residue, product dehydration difficulty, etc., and achieve the effect of reducing dehydration load

Active Publication Date: 2010-05-05
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses ethanol water or methanol crystallization, the product is difficult to dehydrate and may have methanol residue

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Take 100 g of total ginkgo lactones (including 56.3% GA content and 31.2% GB content) with a content higher than 97%, vacuum-dry at 80-100°C, crystallize 2-3 times with 10-30 times of absolute ethanol to obtain GB ; Merge GB, filter and dry, then recrystallize with absolute ethanol, the amount of ethanol is respectively 20, 30, 50, 50 times of the solute amount; then use supercritical CO 2 Extraction (operating temperature 65°C, pressure 12MPa) to remove trace impurities and solvents; vacuum drying (temperature 60°C, vacuum degree: 0.090MPa, time 48h); to obtain 28.3g of GB with content ≥ 99%.

Embodiment 2

[0048] Take 100 g of total ginkgo lactones with a content higher than 97% (among them, GA content 56.3%, GB content 31.2%), after vacuum drying at 80-100°C, use 10-30 times of absolute ethanol to crystallize 2-3 times, separate GB ; Concentrate the remaining mother liquor to obtain GA, and filter it to dryness; recrystallize with absolute ethanol, and the amount of ethanol is 20, 30, 50, 50 times of the solute amount; then use supercritical CO 2 Extraction (operating temperature 55°C, pressure 14MPa) to remove trace impurities and solvents; vacuum drying (temperature 70°C, vacuum degree: 0.095MPa, time 48h); 51.4g of GA with a content ≥ 99% was obtained.

Embodiment 3

[0050] Take 100 g of total ginkgo lactones with a content higher than 90% (among them, GA content 52.6%, GB content 28.8%), first dissolve with 20 to 40 times of ethanol, add an appropriate amount of acidic alumina to decolorize, and improve the purity of total ginkgo lactones; Vacuum dry at 80-100°C; crystallize 2-3 times with 10-30 times absolute ethanol to obtain GB; combine GB, filter and dry; times; then supercritical CO 2 Extraction (operating temperature 50°C, pressure 15MPa) to remove trace impurities and solvents; vacuum drying (temperature 70°C, vacuum degree: 0.090MPa, time: 48h); 26.7g of GB with content ≥ 97.5% can be obtained.

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PUM

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Abstract

A separation and purification method of ginkgolide A and B monomers takes ginkgolides with larger than or equal to 95% purity as a starting raw material and comprises steps of separation, purification and drying. The purification adopts recrystallization-supercritical CO2 extraction combination technology; firstly monomer GA and GB obtained by crystallizing separation are respectively recrystallized with absolute ethyl alcohol for at least three times according to the ratio of material to liquid 1:5-80, thus obtaining the monomer GA and GB with larger than or equal to 95% purity; and then the supercritical CO2 extraction method is used for respectively extracting the monomer GA and GB with larger than or equal to 95% purity; wherein the extraction pressure is 10-100Mpa and the extraction temperature is 32-150 DEG C. The extraction is repeated for one time to prepare the monomer GA and GB with larger than or equal to 95% purity. According to the weight of the monomer in the staring material, the yield is larger than or equal to 90%. In the invention, no other organic solvent is touched apart from alcohol and CO2; and the method is a green environmental protection technology, has high yield and is particularly suitable for the manufacture of crude drugs.

Description

1. Technical field [0001] The invention relates to a method for obtaining medicinal compounds from plants, specifically a new method for separating and purifying ginkgolide A and ginkgolide B monomers from total ginkgolides. 2. Background technology [0002] Ginkgo biloba extract (GBE) has been included in the Pharmacopoeia of the People's Republic of China (2005 edition). The medicinal GBE produced according to this standard has a total flavonol glycoside content ≥ 24%, and a terpene lactone (based on the total amount of bilobalide, ginkgolide A, ginkgolide B and ginkgolide C) content ≥ 6 %. [0003] Ginkgolides include ginkgolide A (hereinafter referred to as GA), ginkgolide B (hereinafter referred to as GB), ginkgolide C (hereinafter referred to as GC), ginkgolide J, ginkgolide M and bilobalide, etc. It is a unique ingredient of Ginkgo biloba. There are certain differences in the efficacy and function of each monomer in total ginkgolides. GA and GB have significant cu...

Claims

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Application Information

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IPC IPC(8): C07D493/22
CPCY02P20/54
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