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Efficient separation method for preparing 23-acetyl alisol B

A high-efficiency technology of acetyl alisol, applied in the production of steroids, bulk chemicals, organic chemistry, etc., can solve the problems of complicated operation, cumbersome steps, consumption of organic solvents, etc., and achieves high efficiency, simple steps, and easy repeatability. Effect

Active Publication Date: 2012-05-23
FUJIAN ACAD OF MEDICAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method is complex in operation, cumbersome in steps, consumes a large amount of organic solvents, a large amount of manpower and material resources, and the purity obtained is low, which cannot meet the requirements of green industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Embodiment 1 Alisma supercritical CO The preparation of fluid extraction solution

[0013] Weigh 3194.8g of Alisma coarse powder, particle size: 20 mesh, and put it into a 10L extraction tank. The extraction route is: CO2 steel cylinder→cooling system→high pressure pump→extraction kettle→analysis kettle I→analysis kettle II→CO 2 Storage Tank → Loop. The extraction temperature is 40°C and the extraction pressure is 35MPa for 2 hours. When the instrument reaches the set conditions, start timing and cycle the extraction for 2 hours. After the extraction was finished, the extract was released from the analysis kettle I and the analysis kettle II, a total of 127.5g, and the yield of the Alisma alisma extract prepared by the supercritical CO2 fluid extraction method was: 3.99%.

Embodiment 2

[0014] 23-Acetyl alisol B countercurrent chromatographic separation in Alisma in embodiment 2

[0015] The solvent system used is n-hexane-ethyl acetate-methanol-water=3:2:3:2, and the four solvents are arranged in a separatory funnel in proportion, fully shaken for 15 minutes (vigorously), and then stand still for 30 minutes to separate phases. After equilibration, the upper and lower phases were obtained respectively, the upper phase was used as the stationary phase, and the lower phase was used as the mobile phase, degassed by ultrasonic for 30 min, and set aside. Weigh an appropriate amount of sample and fully dissolve it in the lower phase (mobile phase), so that the sample concentration is 20mg / mL, the injection volume is 1ml, the stationary phase and the mobile phase are in a volume ratio of 70:30, and pumped into the high-speed countercurrent at a flow rate of 20mL / min. The chromatographic host spiral tube, the protection pressure is set to 1MPa. When the host spiral ...

Embodiment 3

[0016] Embodiment 3 contains the crystallization and recrystallization of 23-acetyl alisitol B component

[0017] After concentrating the collected 23-acetyl alisitol B component solution, it was analyzed by liquid chromatography that the main component of the solution was 23-acetyl alisitol B. When the solution was left at room temperature for a period of time, colorless needles were precipitated Crystallization, separation of crystallization after centrifugation, recrystallization with acetone-water or methanol-water, and vacuum drying to obtain 2 mg of high-purity 23-acetyl alisitol B monomer, which is more than 99% pure through liquid chromatography analysis The yield of 23-acetyl alisitol B after purification and drying by countercurrent chromatography is: 10%, then supercritical fluid extraction, countercurrent chromatography separation and purification, concentrated crystallization and vacuum drying process, the yield of 23-acetyl alisitol B is 0.40%.

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Abstract

The invention discloses an efficient separation method for preparing 23-acetyl alisol B. Total sterol extractive in rhizoma alismatis is extracted by supercritical CO2 fluid; then the extractive is further separated and purified by a high speed countercurrent chromatography; finally the extractive is refined by a recrystallization method to obtain high purity 23-acetyl alisol B. The method is simple, with high efficiency, easy for repetition and suitable for industrialized production; and the 23-acetyl alisol B prepared by separation has a purity more than 99% and can be used as a quality control contrast sample of the traditional Chinese medicine rhizoma alismatis and as a bulk drug.

Description

technical field [0001] The invention relates to a preparation method of a traditional Chinese medicine active monomer, in particular to a separation preparation method of 23-acetyl alisol B. Background technique [0002] 23-Acetyl alisitol B is the main active ingredient in the traditional Chinese medicine Alisma, and the 2010 edition of the Chinese Pharmacopoeia uses this ingredient as a quality control index for the traditional Chinese medicine Alisma and its decoction pieces, so the market demand for the monomer of this substance will increase greatly. The traditional way to obtain the monomer of this substance is to extract it with a large amount of ethanol first, then elute it with column chromatography, and then obtain it through crystallization and recrystallization. This method is complex in operation, cumbersome in steps, consumes a large amount of organic solvents, a large amount of manpower and material resources, and the purity of the obtained product is low, whi...

Claims

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Application Information

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IPC IPC(8): C07J17/00
CPCY02P20/54
Inventor 林文津徐榕青张亚敏
Owner FUJIAN ACAD OF MEDICAL SCI