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Method for preparing gastrodine

A gastrodin and Gastrodia elata technology, applied in the field of gastrodin preparation, can solve the problems of low gastrodin content, serious pollution, unfavorable large-scale production operations, etc.

Inactive Publication Date: 2010-05-12
南京璇荣贸易有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In the prior art, the extraction and separation method of gastrodin mainly adopts organic solvent method, etc., but the content of gastrodin obtained by these extraction processes is low, the pollution in the production process is serious, and it is unfavorable for large-scale production operations

Method used

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  • Method for preparing gastrodine

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Effect test

Embodiment 1

[0016] Take 10Kg of Gastrodia elata coarse powder, add 60% ethanol for percolation, collect the percolation liquid with a volume 5 times the weight of the medicinal material, filter, recover ethanol under reduced pressure and concentrate to dryness, add methanol to dissolve the residue, inject it into a high-efficiency countercurrent extractor, and use water -methanol-ethyl acetate (1:1:8) solvent system, the lower phase is the stationary phase, the upper phase is the mobile phase, collect the gastrodin segment, concentrate, separate out crystals, separate the crystals, add methanol-ethyl acetate (1: 5) Recrystallization, separation, washing, and drying to obtain 4.2 g of gastrodin, which was detected by HPLC with a purity of 97.8%.

Embodiment 2

[0018] Take 10Kg of Gastrodia elata coarse powder, add 90% ethanol for percolation, collect the percolation liquid of 10 times the volume of the medicinal material, filter, recover ethanol under reduced pressure and concentrate to dryness, add methanol to dissolve the residue, inject it into a high-efficiency countercurrent extractor, and use water -methanol-ethyl acetate (1:1:8) solvent system, the lower phase is the stationary phase, the upper phase is the mobile phase, collect the gastrodin segment, concentrate, separate out crystals, separate the crystals, add methanol-ethyl acetate (1: 10) Recrystallization, separation, washing and drying yielded 6.6 g of gastrodin, which was detected by HPLC with a purity of 98.2%.

Embodiment 3

[0020] Take Gastrodia elata coarse powder 10Kg, add 80% ethanol percolation, collect the percolation liquid of 8 times the volume of the medicinal material weight, filter, recover ethanol under reduced pressure and concentrate to dryness, add methanol to dissolve the residue, inject it into a high-efficiency countercurrent extractor, and use water -methanol-ethyl acetate (1:1:8) solvent system, the lower phase is the stationary phase, the upper phase is the mobile phase, collect the gastrodin segment, concentrate, separate out crystals, separate the crystals, add methanol-ethyl acetate (1: 9) Recrystallization, separation, washing, and drying yielded 6.4 g of gastrodin, which was detected by HPLC with a purity of 99.4%.

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Abstract

The invention relates to a method for preparing gastrodine, which has simple operation, light pollution and little equipment input. The method has the following process steps: taking coarse gastrodine powder; adding 60 to 90 percent ethanol into the coarse powder for percolation; collecting percolate of which the volume is 5 to 10 times the weight of a medical material; filtering, and reclaiming the ethanol at reduced pressure; condensing the percolate to dryness; adding methanol into residue for dissolution; injecting the solution into a high-efficient countercurrent extractor; using a lower phase of a water-methanol-acetic ether (1:1:8) solvent system as a stationary phase and an upper phase as a mobile phase, and collecting and condensing a gastrodine section; precipitating and separating crystal; and adding methanol-acetic ether (1:5-10) into the crystal for recrystallization. The gastrodine prepared by the method has high purity and is easy to realize industrialized amplification.

Description

technical field [0001] The invention relates to a method for preparing gastrodin, in particular to a method for extracting gastrodin from plants. Background technique [0002] Gastrodin, synonym: gastrodin. Molecular formula: C13H1807, molecular weight: 286.281, CAS registration number: 62499-27-8, structural formula as follows: [0003] [0004] Gastrodin is a natural compound with various physiological activities such as sedative, hypnotic, and anticonvulsant. It mainly exists in the orchid plant Gastrodia elata Blume. [0005] The traditional Chinese medicine Gastrodia elata is the dry tuber of the orchid plant Gastrodia elata Blume, which has the effect of calming the liver, relieving wind and relieving spasm, and contains a large amount of gastrodin. [0006] In the prior art, the extraction and separation methods of gastrodin mainly use organic solvent methods, etc., but the content of gastrodin obtained by these extraction processes is low, the pollution in the p...

Claims

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Application Information

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IPC IPC(8): C07H15/203C07H1/08
Inventor 张发成毛志英范淦彬
Owner 南京璇荣贸易有限公司
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