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Manufacturing technology for extracting ginkalide A and C from root and bark of maidenhair tree

A technology of ginkgolide and production process is applied in the field of production technology for extracting ginkgolide A and C, and achieves the effects of high separation efficiency, strong durability, and simple and convenient production process operation.

Active Publication Date: 2012-08-22
盐城技源药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve some unsatisfactory problems in the process of extracting ginkgolides, the present invention provides a production process for separating and purifying ginkgolides A and C from the root bark of the ginkgo tree. , Ginkgolide A and C with a purity of 92%, the yield of Ginkgolide A > 0.04%, and the yield of Ginkgolide C > 0.02%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: 10kg of dried ginkgo root bark is cut into 1-3cm. Add 60-75L of 33-35% ethanol for reflux extraction twice, each time for 2-3 hours. Combine the extracts, filter while hot, concentrate in vacuum, control the vacuum at -0.80--0.96Mpa, control the volume after concentration at 1 / 3-1 / 4 of the original volume, add a small amount of ethanol, and adjust the concentration to 3-5%. After cooling down to 40-45 degrees Celsius, add 10-15L ethyl acetate three times, stir and extract, separate and combine the light phases. Ethyl acetate was recovered to dryness. The concentrated intermediate was stirred and dissolved with 400-500ml of 80% ethanol, and filtered to clarify after dissolution. Add an equal amount of purified water to dilute the ethanol concentration to 40% to obtain a column solution. Take the adsorption column and fill it with 4L model: PRP512C high-performance chromatography resin according to the diameter-to-length ratio of 1:5-10, wash the resin co...

Embodiment 2

[0018] Embodiment 2: 10kg of dried ginkgo root bark is cut into 1-3cm. Add 75L of 35% ethanol to reflux for extraction twice, each time for 2-3 hours. Combine the extracts, filter while hot, concentrate in vacuum, control the vacuum at -0.80--0.96Mpa, control the volume after concentration at 1 / 3-1 / 4 of the original volume, add a small amount of ethanol, and adjust the concentration to 3-5%. After cooling down to 40-45 degrees Celsius, add 15L of ethyl acetate three times, stir and extract, separate and combine the light phases. Ethyl acetate was recovered to dryness. The concentrated intermediate was stirred and dissolved with 500ml of 60% ethanol, and filtered for clarification. Add an equal amount of purified water to dilute the ethanol concentration to 30% to obtain a column solution. Take the adsorption column loaded with 4L model: PRP512C high-efficiency chromatography resin. According to the flow rate of 33 ~ 35ml / min, the column solution is sent to the adsorption c...

Embodiment 3

[0019] Embodiment 3: 10kg of dried ginkgo root bark is cut into 1-3cm. Add 75L of 35% ethanol for reflux extraction three times, each time for 2-3 hours. Combine the extracts, filter while hot, concentrate in vacuum, control the vacuum at -0.80--0.96Mpa, control the volume after concentration at 1 / 3-1 / 4 of the original volume, add a small amount of ethanol, and adjust the concentration to 3-5%. After cooling down to 40-45 degrees Celsius, add 15L of ethyl acetate three times, stir and extract, separate and combine the light phases. Ethyl acetate was recovered to dryness. The concentrated intermediate was stirred and dissolved with 500ml of 60% ethanol, and filtered for clarification. Add an equal amount of purified water to dilute the ethanol concentration to 30% to obtain a column solution. Take the adsorption column loaded with 4L model: PRP512C high-efficiency chromatography resin. According to the flow rate of 33 ~ 35ml / min, the column solution is sent to the adsorptio...

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Abstract

The invention relates to a manufacturing technology for extracting ginkalides A and C from roots and barks of maidenhair trees, comprising the following steps of: drying roots and barks of maidenhair trees; refluxing and extracting 35 percent of ethanol; concentrating in vacuum; leaching ethyl acetate for three times; recovering a solvent; dissolving and filtering 60-80 percent of ethanol; then, purifying a chromatogram by using PRP512C inverted chromatographic resin; analyzing diluted alcohol; receiving corresponding effective components and fractions; concentrating in vacuum; respectively using 30 percent of ethanol and 60 percent of ethanol; and recrystallizing three times according to 1:8-15. The manufacturing technology for extracting ginkalides A and C from roots and barks of maidenhair trees has simple and convenient operation, good repeatability and high yield, is suitable for industrialized production and does not contain toxic solvents.

Description

technical field [0001] The invention belongs to a process for extracting medicines from plants, in particular to a process for extracting ginkgolides A and C from ginkgo tree root bark. Background technique [0002] Ginkgolide components are mostly extracted and separated from Ginkgo biloba leaves in various literatures and patent reports at home and abroad. Zhou Guozhu et al. The process is to extract ginkgo leaves or ginkgo root bark with water, separate with activated carbon or macroporous resin, concentrate and precipitate to obtain a lactone mixture. [0003] CN101134758A "Technology for Extracting and Separating Ginkgolides A, B, C, J and Bilobalide Monomer from Ginkgo Leaf", using ethanol to extract ginkgo leaves, ethyl acetate extraction, non-polar resin column adsorption, ethanol crystallization, silica gel Column chromatography, different concentrations of recrystallization separation to obtain bilobalide, ginkgolide A, B, C, J each monomer. [0004] CN1634925A "...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/22
Inventor 李五洲蒋永红曹礼群李新晴张艳李慧芳曹如
Owner 盐城技源药业有限公司
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