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Separation and purification method of ginkgolide A and B monomer

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

Active Publication Date: 2012-01-11
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  • Summary
  • 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 100g of Ginkgo biloba total lactones (including 56.3% GA content and 31.2% GB content) with a content higher than 97%, vacuum-dried at 80-100°C, and crystallize it with 10-30 times absolute ethanol for 2 to 3 times to obtain GB ; Combine GB, filter to dryness, and recrystallize with absolute ethanol. The amount of ethanol is 20, 30, 50, and 50 times the dissolved mass; then 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); obtain 28.3g GB with a content of ≥99%.

Embodiment 2

[0048] Take 100g of Ginkgo biloba total lactones (including 56.3% GA content and 31.2% GB content) with a content higher than 97%, vacuum-dry at 80-100°C, crystallize with 10-30 times absolute ethanol for 2 to 3 times, and separate the GB ; Concentrate the remaining mother liquor to obtain GA, filter it dry; recrystallize with absolute ethanol, the amount of ethanol is 20, 30, 50, 50 times the dissolved mass; 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 content ≥99% is obtained.

Embodiment 3

[0050] Take 100g of total ginkgo lactones (including 52.6% of GA content and 28.8% of GB content) with a content of more than 90%, first dissolve it with 20-40 times ethanol, add an appropriate amount of acidic alumina to decolor, and improve the purity of total ginkgo lactones; Dry under vacuum at 80~100℃; crystallize 2~3 times with 10~30 times anhydrous ethanol to obtain GB; combine GB and filter to dryness; recrystallize with anhydrous ethanol. The amount of ethanol is 20, 40, 60 of the dissolved mass. Times; then use supercritical CO 2 Extraction (operating temperature 50℃, pressure 15MPa) to remove trace impurities and solvents; vacuum drying (temperature 70℃, vacuum degree: 0.090MPa, time: 48h); obtainable GB 26.7g with a content of ≥97.5%.

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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 thesupercritical 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 ginkgo lactones. 2. Background technology [0002] Ginkgo biloba extract (GBE) has been listed in the Pharmacopoeia of the People's Republic of China (2005 edition). The medicinal GBE produced according to this standard has the content of total flavonol glycosides ≥24% and the content of terpene lactones (based on the total amount of bilobalide, ginkgolides A, ginkgolides B and ginkgolides 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, Ginkgolide, etc. It is a peculiar ingredient of Ginkgo. There are certain differences in the efficacy and functions of the monomers in total ginkgo lactones. GA and GB have si...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/22
CPCY02P20/54
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