Process for extracting 4',6'-dihydroxy-3',5'-dimethyl-2'-methoxychalcone from cleistocalyx operculatus flower buds

Abstract

A process for extracting 4',6'-dihydroxy-3',5'-dimethyl-2'-methoxychalcone from cleistocalyx operculatus flower buds comprises steps as follows: step one, dried cleistocalyx operculatus flower buds are ground into coarse powder, 70% (v / v) of ethanol is added for soaking the coarse powder, then the mixture is filtered and subjected to decompressing concentration to dry to obtain yellow dry powder, the solvent is recovered for soaking the powder again, the extraction is performed for three times, and the dry powder obtained through the three times of extraction is combined to obtain crude extract; step two, the crude extract obtained in the step one is directly sampled on a silica gel chromatographic column without dissolving or silica gel addition, and is eluted by utilizing an ether and ester mixed system as a mobile phase, part of eluent is collected and subjected to decompressing concentration to dry, and orange red solid, namely a crude product of chalcone, is obtained; step three, the crude product of chalcone obtained in the step two is recrystallized by absolute methanol at the temperature of 70 DEG C, and the purity is up to or higher than 97.8%; a refined product of chalcone is obtained. According to the process, the purity of chalcone in part of the elution sections of ethyl acetate with certain concentration is up to or higher than 97%, and the stability is good.

Description

technical field [0001] The invention relates to a preparation method for extracting active ingredients from plants, to be precise, a method for preparing 4′,6′-dihydroxy-3′,5′-dimethyl-2′-methanol from water weng flower buds Chromatographic extraction process of oxychalcones. Background technique [0002] The flower buds of water weng are the flower buds of Cleistocalyx operculatus (Roxb.) Merr. Et Perry, a plant of Myrtaceae. Shuiwenghua, also known as Shuixiang, Jiuweng, and Hibiscus bark, is distributed in Guangdong, Hainan, Guangxi, Yunnan and other places. It likes warm and humid climates and often grows next to water. Slightly fragrant, bitter, and cold in nature, it is often used as herbal tea in Guangdong folks. It has the effects of clearing heat and detoxifying, digesting stagnation, and is widely used among folks. It is also the main raw material of "heat-clearing herbal tea" Chinese patent medicine. [0003] Modern research shows that flower buds contain active...

AI Technical Summary

Problems solved by technology

[0004] At present, the extraction and purification of flavonoids mainly use silica gel column chromatography, macroporous resin, dextran gel chromatography and other solid-liquid chromatography for repeated elution and separation. Repeated elution and separation will cause serious loss of samples. It is also difficult to obtain high-purity monomers after repeated separations, or the amount obtained is very small, which cannot meet the follow-up related research on activity, drug efficacy and pharmacological effects, and it takes a long time and consumes a lot of eluent.