Method for separating and purifying carnosic acid from rosemary extract through atmospheric pressure column chromatography

Abstract

Provided is a method for separating and purifying carnosic acid from rosemary extract through atmospheric pressure column chromatography. Silica gel is evenly dispersed though petroleum ether with the volume equal to that of the silica gel at the temperature ranging from 60 DEG C to 90 DEG C and then homogenate wet-method packing is performed, the rosemary extract is dissolved through butyl acetate and then added into a sample, butyl acetate and petroleum ether are mixed according to the volume ratio of 4:1 to 4:10 at the temperature ranging from 60 DEG C to 90 DEG C and serve as eluent, the flow speed is 2 mL / min to 8 mL / min, segmented fraction collection is performed after elution, the fractions of the same content are combined, a chromatography product is obtained through vacuum concentration, and the carnosic acid product with the purity higher than 98% can be obtained. According to the method, a convectional solvent easy to obtain is used, no special high-pressure and high-temperature devices are needed, cost is low, the purifying efficiency is high, and the residual solvent is small and can be recycled easily.

Description

technical field [0001] The invention relates to a method for separating and purifying carnosic acid from rosemary extract by normal pressure column chromatography, in particular to a method for separating and purifying carnosic acid from rosemary extract by normal pressure silica gel column chromatography A preparation method for purifying carnosic acid. Background technique [0002] The purification methods of carnosic acid mainly include buffer solution purification method, pH value control precipitation method, and column chromatography purification method. The column chromatography purification method, medium pressure or normal pressure column is the most used. [0003] The buffer solution refining process is simple and easy to operate, but the purity of the obtained carnosic acid is not enough; the pH control precipitation method purifies the carnosic acid, and the purity of the obtained product can meet certain requirements, but the process is complicated and takes a l...

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Problems solved by technology

[0003] The buffer solution refining process is simple and easy to operate, but the purity of the obtained carnosic acid is not enough; the pH control precipitation method purifies the carnosic acid, and the purity of the obtained product can meet certain requirements, but the process is complicated and takes a long time, and the experimental requirements are very low temperature to ensure the freezing and crystallization of carnosic acid, which consumes a lot of energy; column chromatography is widely used, and the rosemary antioxidant crudely extracted by various solvents is dissolved in dichloromethane and separated by a polyamide column, and then passed through two Sub-recrystallization and activated carbon decolorization can obtain the colorless crystals of carnosic acid with a purity greater than 95% (Sun Chuanjing, Sun Yunpeng. Supercritical CO 2 The method of extracting rosemary antioxidant by reverse extraction method: China, 1327038 [P].2001-12-19), but the purification time is long, and the purification cost is high; adopt RP-C18 filler to separate and purify the rosemary extract Carnosic acid can be obtained with a purity of more than 98% (Du Jiquan, Xu Hong, Chen Xiangxue, etc. Separation and purification of carnosic acid in rosemary and determination of antioxidant capacity index [J]. Food and Machinery, 2011,27(6):87-91); using carnosic acid raw materials with a content of not less than 15% to prepare carnosic acid with a purity of more than 98%, dissolving the crude carnosic acid in butyl acetate to obtain a column sample , use silica gel to fill the column, after loading the sample, use butyl acetate as the eluent, plunger solvent pump into the liquid, collect the eluted fractions in sections, concentrate under reduced pressure to dryness and recover the eluent, and obtain the chromatographic product , the chromatographic product is recrystallized with a hydrocarbon solvent, and the crystallized product is dried under reduced pressure to obtain a carnosic acid product with a purity of more than 98% (Zu Yuangang, Yang Lei, Zu Baishi, etc. A continuous medium-pressure column chromatography to prepare high Purity method of carnosic acid: China, 101851158A[P].2010-10-06.)

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