Purification method of gastrodin

A purification method and gastrodin technology, which is applied in the field of refining gastrodin by ODS reversed-phase silica gel method, can solve the problems of difficult handling of the extract, easy gelatinization of starch, etc., and achieve the effects of reducing starch dissolution, easy handling, and preventing gelatinization

Inactive Publication Date: 2011-11-23
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The starch in Gastrodia elata is easily gelatinized by heat reflux extraction, and the extract is difficult to handle

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take 1 kg of Gastrodia elata powder, add 5 L of 40% methanol solution to reflux and extract twice, extract for 1 hour each time, recover the solvent from the extract until it has no alcohol smell, purify it with polyamide resin, and wash it with water, 20% and 60% ethanol aqueous solution respectively Remove, collect 20% and 60% eluents, combine and concentrate, then take 450g ODS silica gel to pack into the column, take another 50g ODS silica gel and concentrate to mix the sample, evaporate the solvent, put on the column, elute with 60% methanol aqueous solution, collect and elute liquid, concentrated and dried to obtain 8.3g of the product, with a content of 99.1%.

Embodiment 2

[0020] Take Gastrodia elata medicinal powder 1kg, add 12L of 70% ethanol solution to reflux and extract 4 times, extract for 3 hours each time, recover the solvent from the extract until it has no alcohol smell, purify it with polyamide resin, and use 20%, 40% and 60% ethanol aqueous solution respectively Gradient elution, collect 40% and 60% eluents, combine and concentrate, then take 1000g ODS silica gel to pack into the column, take another 125g ODS silica gel and concentrate to mix the sample, evaporate the solvent, put on the column, elute with 55% acetonitrile aqueous solution, collect The eluate was concentrated and dried to obtain 10.1 g of the product with a content of 99.3%.

Embodiment 3

[0022] Take 5 kg of Gastrodia elata medicinal powder, add 40 L of 50% ethanol solution to reflux and extract 3 times, extract for 2 hours each time, recover the solvent from the extract until it has no alcohol smell, purify it with polyamide resin, and use 10%, 30% and 50% ethanol aqueous solution respectively Gradient elution, collect 20-40% and 40-60% eluents, combine and concentrate, then take 3kg ODS silica gel to pack the column, take another 300g ODS silica gel and concentrate, mix the sample, evaporate the solvent, put it on the column, and use 70% methanol aqueous solution After elution, the eluate was collected, concentrated and dried to obtain 45.7 g of the product, with a content of 98.7%.

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Abstract

The invention relates to a purification method of gastrodin. The method comprises the following specific steps: (1) using an alcohol-containing solution to perform ultrasonic extraction on gastrodin medicinal herb powder, collecting extract, concentrating to ensure that the extract has no alcohol; and (2) purifying a concentrated solution with polyamide resins, adopting ethanol-water (0-60%) to perform gradient elution, collecting the target eluent, concentrating to reach a small volume, adopting the dry method to add the concentrated target eluent with a small volume into an octadecylsilyl (ODS) silica gel column, eluting with an ethanol-water mixed solvent or an acetonitrile-water mixed solvent, recycling the solvent from the eluent, and drying to obtain gastrodin. The method has the advantages of low energy consumption, short preparation period and high product purity.

Description

technical field [0001] The invention belongs to the field of natural product separation, and in particular relates to a method for refining gastrodin by using an ODS reversed-phase silica gel method. Background technique [0002] Gastrodia elata is the orchid plant Gastrodia elata ( Gastrodia elata Bl.) dry tubers. Gastrodia elata has the effects of calming the liver, relieving wind and relieving convulsions, and is used to treat headaches, dizziness, limb numbness, convulsions in children, epilepsy, convulsions, and tetanus. Studies have shown that the main active ingredient of Gastrodia elata is gastrodin compounds, among which gastrodin has analgesic, sedative and increased cerebral blood flow, reduces cerebral blood flow resistance, especially can increase the blood supply of vertebrobasilar artery, improve labyrinthine artery and inner ear The role of blood supply is often used as an index component for the quality control of Gastrodia elata medicinal materials. Stud...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/203C07H1/08
Inventor 刘东锋吴艳波
Owner NANJING ZELANG MEDICAL TECH
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