Process for preparing nobiletin based on multiple solvents

Abstract

The invention discloses a process for preparing nobiletin based on multiple solvents. Any one or more of dried tangerine or orange peel (orange peel), fruits of immature citrons, fructus aurantii (bitter oranges) and shaddock peel are adopted as raw materials, the raw materials are smashed into coarse powder firstly, then methyl alcohol or ethyl alcohol with the volume concentration of 50%-95% is adopted as a solvent, and extraction is conducted through a percolation method or a reflux extraction method or an impregnation method; after an extracting solution is collected, vacuum concentration is conducted, and extract without the alcohol taste is obtained; the extract obtained after alcohol extraction is chloroformed with an organic solvent or extracted with ethyl acetate firstly, extractant is concentrated and then repeatedly extracted with a ternary two-phase solvent system formed by acetone, petroleum ether and water, the lower layer of the extractant which is repeatedly extracted is concentrated, coarsely crystallized and repeatedly recrystallized, and nobiletin crystals with the purity of 98% or above are obtained. The obtained nobiletin can be used for quality control over national standard substances/medicinal materials and decoction pieces or quality monitoring on Chinese patent medicine, and compared with the prior art, the process has the advantages of being simple in technological process, practical, low in cost, high in purity and yield and suitable for industrial production.

Description

technical field [0001] The invention relates to a method for separating and preparing monomer components in traditional Chinese medicine, in particular to a process for preparing nobietin based on multi-solvent. Background technique [0002] Tangerine peel, citrus aurantium, citrus aurantium, and pomelo peel are all commonly used traditional Chinese medicines in clinical practice of traditional Chinese medicine. class etc. Nobiletin is a colorless crystal extracted from the above medicinal materials, with a melting point of 137-138°C; slightly soluble in water and ether; the molecular formula is C 21 h 22 o 8 ; Molecular weight 402.39. The structural formula is as follows: [0003] . [0004] Nobiletin (Naringenine-7-rhamnosidoglucoside) English name Nobiletin, also known as Chuanpiting, Tangerine, is a colorless crystal, belonging to a polymethoxy flavonoids. [0005] Nobiletin has anti-hemagglutination, anti-thrombosis, anti-cancer, anti-fungal, anti-inflammatory,...

AI Technical Summary

Problems solved by technology

[0007] The object of the present invention is to provide a kind of technology that prepares nobiletin based on multi-solvent, to overcome the defects such as complicated steps, long separation time, poor separation ability and low purity of nobiletin in the separation method of nobiletin in the prior art