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

A technology of rosemary extract and carnosic acid, which is applied in the field of separation and purification of carnosic acid, can solve the problems of insufficient purity of carnosic acid, long purification time, and high purification cost, so as to improve the utilization rate of raw materials and equipment, Inexpensive, less residue effect

Inactive Publication Date: 2014-09-24
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Abstract
  • Description
  • Claims
  • Application Information

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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 Carn

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

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Preparation method of rosemary extract powder (Li Dawei. Ultrasonic-assisted extraction and separation of active components of rosemary leaves [D]. Beijing: Chinese Academy of Forestry Master's degree thesis, 2012): 100g rosemary leaves (crushing), add 75% ethanol 1600mL according to solid-liquid ratio 1:16 (g / mL), add 3% acid stabilizer (relative to ethanol), ultrasonic frequency 28kHz, ultrasonic power 200W, ultrasonic extraction time 40min, ultrasonic temperature 35°C. The extract is filtered to obtain a filtrate, and the filtrate is distilled under reduced pressure to obtain a rosemary extract extract, which is dried in a vacuum oven at 40°C and ground in a mortar to obtain 16.93 g of rosemary extract powder (the carnosic acid content is 20%wt).

Embodiment 2

[0020] Rosemary extract powder (prepared according to the method of Example 1, carnosic acid content is 20%wt, the same below.) 0.5g, dissolved with 1-2mL butyl acetate, to get the column sample. Weigh 40 g of 200-300 mesh silica gel, disperse it with an equal volume of petroleum ether (60-90° C.), and then homogenate it for wet packing. Put half a column of petroleum ether (60-90°C) into the chromatography column, and slowly add silica gel. Rinse with petroleum ether (60-90°C) to fully settle the packing, and tap the side wall of the chromatography column to make the packing compact and uniform. The eluent is butyl acetate: petroleum ether (60-90°C) at a ratio of 4:10 (v / v), the flow rate is 6mL / min, and the sampling volume is 5mL / tube. It is separated by column chromatography and identified by thin-layer chromatography. Several fractions with higher carnosic acid content were collected and combined, concentrated to dryness under reduced pressure to obtain 0.0642 g of a puri...

Embodiment 3

[0022] 0.5 g of rosemary extract powder was dissolved in 1-2 mL of butyl acetate to obtain a column sample. Weigh 40 g of 200-300 mesh silica gel, disperse it with an equal volume of petroleum ether (60-90° C.), and then homogenate it for wet packing. Put half a column of petroleum ether (60-90°C) into the chromatography column, and slowly add silica gel. Rinse with petroleum ether (60-90°C) to fully settle the packing, and tap the side wall of the chromatography column to make the packing compact and uniform. The eluent is butyl acetate:petroleum ether (60-90°C) at a ratio of 4:11 (v / v), the flow rate is 6mL / min, the sample volume is 5mL / tube, separated by column chromatography, and identified by thin-layer chromatography Several fractions with higher carnosic acid content were collected and combined, concentrated to dryness under reduced pressure to obtain 0.0726 g of a purified product of carnosic acid.

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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...

Claims

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Application Information

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IPC IPC(8): C07C62/32C07C51/47
CPCC07C51/47
Inventor 毕良武夏田娟赵振东程贤
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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