Adsorption resin method separation technology of scutellarin in fleabane flower extract

Abstract

The invention discloses an adsorption resin method separation technology of scutellarin in a fleabane flower extract. Based on scutellarin and fleabane flower essence A which have very similar structures, the difference of intermolecular hydrogen bonding capacities is formed, an amide functional group capable of forming hydrogen bonds is introduced on a macroporous adsorption resin skeleton, highly selective adsorption is carried out on the scutellarin by the synergic action of dewatering and the hydrogen bonds, a commercially available extract is used as a raw material, and a specimen with the content of the scutellarin more than 98% and the content of the fleabane flower essence A less than 0.5% is prepared by a one-step continuous technology of adsorption and desorption. The invention avoids using a poisonous organic solvent with low boiling point and does not need the assistance of other purification methods, so that the invention has simple operation and is environment-friendly, resin can be recycled simultaneously, the production cost is greatly reduced, and the invention is suitable for large-scale industrial production. The obtained specimen can meet the requirements for further enhancing the quality standard of a breviscapine preparation, reducing clinical side reactions and the like, and the invention has favorable application prospect.

Description

【Technical field】: [0001] The invention belongs to the technical field of separation and purification of monomeric active ingredients in natural plants. In particular, the adsorption separation process of two monomer components with very similar structures in the scutellarin extract - scutellarin and scutellarin, and the synthesis method of the highly selective adsorption resin used in the separation process. 【Background technique】: [0002] Erigeron breviscapus (Vant.) Hand.Mazz. is the dry whole plant of the genus Erigeron breviscapus (Vant.) Hand.Mazz. in the family Asteraceae. It is mainly distributed in Yunnan, Guangxi and other provinces in southwest my country. . Scutellarin is the main flavonoid active ingredient in the extract of scutellarin, which has obvious protective effects on the heart, brain, liver and kidney. Various preparations using breviscapine extracts as raw materials have been widely used clinically, such as the treatment of hypertension, coronary he...

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Problems solved by technology

However, since the commercial adsorption resin skeleton is still dominated by polystyrene, the structure is single, and the adsorption mechanism is mainly hydrophobic adsorption, which results in relatively poor selectivity of the adsorption separation method.

In the extraction and purification of breviscapine, the macroporous adsorption resin is more used as the enrichment material for the active ingredients with a lower content, and it is difficult to truly remove impurities and prepare high-purity extracts. For example, Lou Yunyan et al. discussed The feasibility of using commercial polystyrene macroporous resins to purify scutellarin, studies have shown that these resins can effectively remove some impurities, but it is difficult to prepare high-purity scutellarin (Lou Yunyan et al., static adsorption method Selection of macroporous resin for purifying breviscapine [J], Journal of Traditional Chinese Medicine, 2006, 24(6): 1129)

Zhang Renwei and others disclosed a Chinese invention patent, which used commercialized AB-8 and D101 macroporous polystyrene-type adsorption resins as separation materials for the further purification of commercially available scutellarin raw materials, and obtained a purity of about 90%. scutellarin, but in the purification process disclosed in the patent, the purity of scutellarin in the desorption solution obtained only through the resin "adsorption-desorption" one-step process is difficult to meet the requirements, and the pH value of the desorption solution still needs to be adjusted The scutellarin in it is separated out in the form of precipitation to achieve the purpose of further purification. Therefore, it is difficult to realize the continuous operation process, and the high acidity (pH=1~2) will destroy the structural stability of scutellarin

More importantly, although a large number of impurities were removed after the two-step treatment of resin adsorption and precipitation, the purity of scutellarin increased from 80% to 90%, but due to the adsorption selectivity of AB-8 or D101 resin Poor, it is difficult to realize the separation of scutellarin A and B with similar structure, so using the separation process disclosed in the patent, it is impossible to obtain a scutellarin sample with higher purity and no scutellarin (Zhang Renwei et al. Preparation method of refined scutellarin bulk drug with porous resin, application number 200710065713.6, publication number CN101037461A)

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