Separation and purification method for ginkgolide monomer

A ginkgolide, separation and purification technology, applied in organic chemistry, bulk chemical production and other directions, can solve the problems of single crystal form of monomer, differences in physical and chemical properties and efficacy, and achieve consistent crystal form, efficient production, and simple process. Effect

Inactive Publication Date: 2005-07-06
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0021] In the existing methods for the separation and purification of ginkgolides, the crystal form of the obtained monomer is not guaranteed to be single, and the physical and chemical properties and efficacy of monomers with different crystal forms are often different.

Method used

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  • Separation and purification method for ginkgolide monomer
  • Separation and purification method for ginkgolide monomer
  • Separation and purification method for ginkgolide monomer

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Take 100 g of total ginkgo lactones with a content ≥ 97%, dry them, add them to silica gel column chromatography, use petroleum ether-ethyl acetate mixed solvent as mobile phase (mixing ratio is 90:10~10:90), gradient elution, and collect Ginkgolide B (GB) fractions with a purity of ≥50%; vacuum concentrate the GB fractions to dryness to obtain crude GB; recrystallize with ethanol water; then use supercritical CO 2 Refining and purification (operating temperature 32-100°C, pressure 10-100MPa, extraction and crystallization) to remove trace impurities and solvents, and control the crystal form; drying; to obtain GB15-25g with a content greater than 99% (with the total ginkgo lactones in the raw material The content of GB is different, and the yield varies); the total yield is more than or equal to 90%.

Embodiment 2

[0036] Get 100g of total ginkgolides with a content ≥ 97%. Add it to silica gel column chromatography after drying, use petroleum ether-ethyl acetate mixed solvent as mobile phase (mixing ratio is 90:10~10:90), gradient elution, collect the ginkgolide A (GA ) fraction. The GA fraction was concentrated to dryness in vacuo to obtain crude GA. Recrystallize with ethanol-acetic acid-water, and then use supercritical CO 2 Refining and purification (operating temperature 32-150°C, pressure 10-100MPa) to remove trace impurities and solvents, and control the crystal form; drying; the highest content of 99.8% GA20-25g can be obtained (with GA in the total ginkgo lactone raw material The content is different, and the yield varies); the total yield is more than or equal to 85%.

Embodiment 3

[0038] Get 100g of total ginkgolides with a content ≥ 97%. After drying, add it to reverse-phase silica gel column chromatography, use methanol-water mixed solvent as mobile phase (mixing ratio is 95:5 ~ 5:95), gradient elution, and collect ginkgolide B (GB) with a purity of ≥50%. flow portion. The GB fraction was concentrated to dryness in vacuo to obtain crude GB. Recrystallization from methanol and water followed by supercritical CO 2 Refining and purification (operating temperature 32~150°C, pressure 10~100MPa), to remove trace impurities and solvents, and control the crystal form; dry; get GB25~35g with a content greater than 99% (with the content of GB in the total ginkgo lactone raw material Different, the yield varies); the total yield ≥ 90%.

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Abstract

A separation and purification process for bilobalide monomers is provided. The column chromatography-recrystallization-supercritical CO2 refinement purification combined process is adopted to prepare high purity bilobalide monomers. The column chromatography adopts positive or reverse fixed packing material. Water and ethyl acetate are used for gradient elution. Supercritical CO2 is used for refinement purification and crystallographic form arrangement. The process conditions are: the pressure is less than or equal to 100Mpa, and the temperature is less than or equal to 150 Celsius degrees. The obtained monomers content amounts to 99.8% at the utmost, and the total yield is greater than or equal to 90%.

Description

1. Technical field [0001] The invention relates to a method for separating and purifying various monomeric active components from plant extracts, specifically a method for separating and purifying ginkgolide monomers from ginkgo biloba extracts. 2. Background technology [0002] The composition of Ginkgo biloba is extremely complex, containing a variety of active ingredients, mainly flavonoids, terpene lactones, organic acids, alkylphenols and alkylphenolic acids, steroidal compounds, trace elements, etc. The medicinal ingredients in Ginkgo biloba are mainly ginkgo flavonoids and ginkgolides. [0003] Ginkgo biloba extract (GBE) has been included in the Pharmacopoeia of the People's Republic of China (2000 edition, supplement). Currently, the medicinal GBE produced according to this standard has a content of total ginkgo flavonoids ≥ 24%, and a content of total ginkgo lactones ≥ 6%. [0004] The total ginkgo lactones include ginkgolides A, B, C, J, M and bilobalide, which ...

Claims

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Application Information

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