Method for separating and purifying orlistat

A technology for separation and purification of orlistat, applied in the field of preparation of raw materials, can solve the problems of low production efficiency and yield, high cost, and inability to meet industrial large-scale production, and achieve low cost, simple operation, and short purification time Effect

Inactive Publication Date: 2018-10-16
JIANGSU HANBON SCI & TECH CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, low-pressure column chromatography and crystallization are generally used to purify pure orlistat, but the production efficiency and yield are low, and the cost is high, which cannot meet the needs of large-scale industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] The crude orlistat was dissolved in acetonitrile, filtered with a 0.45um microporous membrane, the mobile phase was acetonitrile:methanol=6:4, phenylsilane bonded silica gel was used as the stationary phase, the particle size of the filler was 20 um, and after loading the sample was about After 50 minutes, the target component was received, and the collection time was 18 minutes. After the collected target fraction was processed by a rotary evaporator, the obtained white powder was pure orlistat, and the purity was 99.2% after testing.

Embodiment 2

[0014] The crude orlistat was dissolved in acetonitrile, filtered with a 0.45um microporous membrane, the mobile phase was acetonitrile:methanol=6:4, octylsilane bonded silica gel was used as the stationary phase, the particle size of the filler was 30 um, and after loading the sample was about After 50 minutes, the target component was received, and the collection time was 18 minutes. After the collected target fraction was processed by a rotary evaporator, the obtained white powder was pure orlistat, and the purity was 99.3% after testing.

Embodiment 3

[0016] The crude orlistat was dissolved in acetonitrile and filtered with a 0.45um microporous membrane. The mobile phase was acetonitrile:methanol=6:4, butylsilane bonded silica gel was used as the stationary phase, and the particle size of the filler was 50 um. After about 50 minutes, the target component was received, and the collection time was 18 minutes. After the collected target fraction was processed by a rotary evaporator, the obtained white powder was pure orlistat, and the purity was 99.1% after testing.

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Abstract

The invention discloses a method for separating and purifying orlistat. Pure orlistat is prepared through separation by using a high pressure preparative liquid chromatography system with bonded silica gel filler as a stationary phase and acetonitrile and methanol as a flowing phase. The method is simple in operation and short in purification time, and the purity of a target product reaches up to99% or above.

Description

technical field [0001] The invention relates to a method for purifying pure orlistat, which belongs to the field of preparation of raw materials. Background technique [0002] Orlistat, the English name is Orlistant, white powder, odorless, tasteless, insoluble in water, easily soluble in acetonitrile, methanol, n-heptane and other organic solvents. Orlistat, as a gastrointestinal lipase inhibitor, is mainly used clinically for the treatment of overweight and obesity. At present, low-pressure column chromatography and crystallization are generally used to purify pure orlistat, but the production efficiency and yield are low, and the cost is high, which cannot meet the needs of large-scale industrial production. [0003] High-pressure preparative liquid chromatography, a liquid chromatography preparation method that uses a high-pressure, large-flow delivery system to perform high-purity separation of samples on a high-resolution, large inner diameter, and high-load separatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D305/12
CPCC07D305/12
Inventor 陈海范大双韩海峰严忠张明亮尤慧艳
Owner JIANGSU HANBON SCI & TECH CO
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