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Orlistat industrial liquid chromatogram preparation method

A technology of orlistat and chromatographic system, which is applied in the field of preparation of orlistat, can solve the problems of long time and low purity, and achieve the effect of easy control and simplified process technology

Inactive Publication Date: 2014-05-14
江苏汉邦科技股份有限公司
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a new method for preparing high-purity orlistat using an industrial preparation-grade liquid chromatography separation system for the problems of long time and low purity in the crude orlistat refining process. , the method includes the following steps:

Method used

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  • Orlistat industrial liquid chromatogram preparation method
  • Orlistat industrial liquid chromatogram preparation method
  • Orlistat industrial liquid chromatogram preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0013] 1. Take 1g of crude orlistat and mix it with 80% methanol solution to prepare a 5% sample solution, put it in a filter device, and filter to remove solid particles;

[0014] 2. Inject the orlistat solution into a dynamic axial compression column to prepare a chromatographic system. The dynamic axial compression column size is Φ50×250mm, the octadecyl reversed-phase silica gel particle size is 10μm, the sample volume is 1g, and the flow rate of the mobile phase is It is 80ml / min. The volume ratio range of mobile phase methanol to water is 80 / 20, elution takes 45 minutes, and one separation cycle ends. The detection wavelength of the ultraviolet photometric detector that adopts is 195nm, collects the cut that retention time is in 33~40min, as figure 2 Shown, through HPLC analysis purity ≥ 99.5%.

Embodiment 2

[0016] 1. Take 1g of crude orlistat and mix it with 80% methanol solution to prepare a 5% sample solution, put it in a filter device, and filter to remove solid particles;

[0017] 2. Inject the orlistat solution into a dynamic axial compression column to prepare a chromatographic system. The dynamic axial compression column size is Φ50×250 mm, the particle size of the octane reversed-phase silica gel filler is 10 μm, the sample volume is 1 g, and the flow rate of the mobile phase is 80ml / min. The volume ratio of mobile phase methanol to water is 78 / 22, elution takes 60 minutes, and one separation cycle ends. The detection wavelength of the ultraviolet photometric detector that adopts is 195nm, collects the cut that retention time is in 40~48min, as image 3 Shown, through HPLC analysis purity ≥ 99.6%.

Embodiment 3

[0019] 1. Take 2g of crude orlistat and mix it with 80% methanol solution to prepare a 5% sample solution, place it in a filter device, and filter to remove solid particles;

[0020] 2. Inject the orlistat solution into the dynamic axial compression column to prepare the chromatographic system. The dynamic axial compression column size is Φ150×250mm, the octadecyl reversed-phase silica gel particle size is 10μm, the sample volume is 2g, and the flow rate of the mobile phase is It is 600ml / min. The volume ratio of mobile phase methanol to water is 78 / 22. After elution for 85 minutes, a separation cycle ends. The detection wavelength of the ultraviolet photometric detector that adopts is 195nm, collects the cut that retention time is in 64~74min, as Figure 4 Shown, through HPLC analysis purity ≥ 99.5%.

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Abstract

The invention discloses an orlistat preparation method, the orlistat synthesis crude product is employed as a raw material, and is performed through a HPLC optimization condition to obtain an appropriate mobile phase and column separating condition, and is amplified to an industrial preparation scale liquid chromatogram separating system for further to obtain the orlistat with high purity. The orlistat industrial liquid chromatogram preparation method has the advantages that industrial preparation scale liquid chromatogram separating system is directely used on the crude product after synthesis to obtain the required substance, so that good separating and purification effects can be reached, the orlistat industrial liquid chromatogram preparation method has the advantages of simple operation, short period and high efficiency, the purity can reach more than 99.5%, and the individual impurity can be controlled below 0.3%.

Description

technical field [0001] The invention belongs to the technical field of biomedicine, and in particular relates to a preparation method of orlistat. Background technique [0002] Orlistat (orlistat) is a gastrointestinal lipase inhibitor, clinically mainly used for the treatment of overweight and obesity. As weight-loss drugs such as fenfluramine and sibutramine have been withdrawn from the market due to serious adverse reactions, orlistat has become the only survivor in the weight-loss drug market due to its unique safety and effectiveness. Generally, low-pressure column chromatography and crystallization are used to purify orlistat, and the production efficiency and yield are low. The present invention purifies orlistat based on a dynamical axial compression (DAC) preparative liquid chromatography, which greatly improves the purification efficiency and yield. Contents of the invention [0003] The purpose of the present invention is to provide a new method for preparing ...

Claims

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Application Information

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IPC IPC(8): C07D305/12
CPCC07D305/12
Inventor 张宇王亚辉初新
Owner 江苏汉邦科技股份有限公司
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