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Preparation method for extracting vanillin from gastrodia tubers

A technology of vanilla aldehyde and ethanol reflux extraction, applied in the separation/purification of carbonyl compounds, organic chemistry and other directions, can solve the problems of large amount of organic solvent, serious pollution, low extraction rate and the like

Inactive Publication Date: 2019-12-06
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional extraction method has the disadvantages of large amount of organic solvent used, serious pollution, and low extraction rate. Using high-speed countercurrent chromatography to separate vanillin can not only gently crush and decompose plant tissue, but also greatly increase the yield. , and it is not easy to destroy the three-dimensional structure of the ingredients

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Take Gastrodia elata, use 3 times the amount of 30% ethanol to reflux extract once, each time for 0.5h, filter, combine the extracts, concentrate until there is no alcohol to obtain a concentrated solution, and add the above concentrated solution to the AB-8 macroporous resin column Adsorption purification, the volume-to-weight ratio of the dosage to the medicinal material is 1:1, and eluted with 4BV of acid alcohol (acid alcohol is a 30% ethanol solution containing 1% acetic acid), collects the eluate, recovers the solvent to dryness, and dissolves the above Gastrodia elata extract was separated by high-speed counter-current chromatography, the parameters were set as: rotating speed 700r / min, mobile phase flow rate 1ml / min, the eluate was collected, concentrated, and dried to obtain high-purity vanillin.

Embodiment 2

[0014] Take Gastrodia elata, use 5 times the amount of 60% ethanol to reflux extract for 3 times, each time for 1.5h, filter, combine the extracts, concentrate until alcohol-free to obtain a concentrated solution, and add the above concentrated solution to the D-101 macroporous resin column Adsorption purification, the volume-to-weight ratio of the dosage to the amount of medicinal materials is 1:3, and eluted with 8BV acid alcohol (acid alcohol is a 50% ethanol solution containing 1% acetic acid), collects the eluate, recovers the solvent to dryness, and dissolves the above Gastrodia elata extract was separated by high-speed counter-current chromatography, the parameters were set as: rotating speed 1000r / min, mobile phase flow rate 5ml / min, the eluate was collected, concentrated, and dried to obtain high-purity vanillin.

Embodiment 3

[0016] Take Gastrodia elata, use 4 times the amount of 50% ethanol to reflux extract 3 times, each time for 1h, filter, combine the extracts, concentrate until alcohol-free to obtain a concentrated solution, add the above concentrated solution to DS-401 macroporous resin column for adsorption For purification, the volume-to-weight ratio of the dosage to the medicinal material is 1:2, elute with 6BV acid alcohol (acid alcohol is a 40% ethanol solution containing 1% acetic acid), collect the eluate, recover the solvent to dryness, and dissolve the above gastrodia elata The extract was separated by high-speed counter-current chromatography with parameters set as: rotating speed 800r / min, mobile phase flow rate 4ml / min, collected eluate, concentrated, and dried to obtain high-purity vanillin.

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Abstract

The invention relates to the technical field of medicines, specifically to an extraction method for vanillin. The extraction method comprises the following steps: (1) pulverizing gastrodia tubers, andcarrying out ethanol reflux extraction; (2) carrying out purification with macroporous resin; (3) performing separation by using a high-speed counter-current chromatograph; and (4) carrying out concentrating and drying to obtain the vanillin. According to the method, the vanillin is extracted through ethanol reflux extraction, macroporous resin purification and high-speed counter-current chromatographic separation; and method is simple in process, short in extraction time, high in extraction rate, low in production cost and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of separation of effective components of natural products, and in particular relates to a method for extracting and purifying vanilla aldehyde in Gastrodia elata. Background technique [0002] Tianma, also known as Chijian, Duyaozhi, Limu, Helicao, Shencao, Guiduyou, Mupu, Mingma, Dingfengcao, Bailongpi, etc., is a perennial herb of the genus Gastrodia in the family Orchidaceae. The rhizome is thick, without green leaves, and the capsule is obovate-elliptic, often propagated by tubers or seeds. Its rhizome is used in medicine to treat dizziness, numbness of limbs, convulsions in children, etc. The main medicinal component is vanillin, and the extraction process of industrially produced vanillin is not perfect, which directly affects the purity of the product and the benefits of industrial production. This paper mainly studies on this, in order to provide reference for improving product purity and industrial producti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/78C07C47/58
CPCC07C45/78C07C47/58
Inventor 杨成东
Owner NANJING ZELANG AGRI DEV