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Method for separating and purifying Orlistat

A technology of orlistat and mobile phase, which is applied in the field of separation and purification, can solve the problems of high sample loss rate, large environmental pollution, and small purification range, and achieve the effects of less solvent consumption, less environmental pollution in operation, and simple process

Active Publication Date: 2012-07-11
SHANDONG NEWTIME PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to overcome the defects of complex process, small purification range, large environmental pollution and high sample loss rate in the existing orlistat purification method, the present invention provides a method for recovering high-purity orlistat from orlistat crude product The separation and purification method has the advantages of simple process, small amount of organic solvent, and high product purity and recovery rate.

Method used

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  • Method for separating and purifying Orlistat
  • Method for separating and purifying Orlistat
  • Method for separating and purifying Orlistat

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Dissolving and filtering:

[0040] According to the ratio of orlistat crude product solid mass:solvent volume=10g:1L, orlistat crude product solid is dissolved with mobile phase, after dissolving, filter with organic microporous membrane of 0.45 μm, the filtrate is prepared as the next step to purify orlistat Raw material of lixistat.

[0041] The purity of the orlistat of the crude product used is 96% (HPLC area normalization method), and the maximum simple impurity is 0.6% (HPLC does not add the principal component self-contrast method of correction factor, Chinese Pharmacopoeia 2010 edition, P appendix 31), flow Phase select methanol-water solution with a volume ratio of 86:14

[0042] (2) separation and purification:

[0043] Inject 2L of the filtrate in step (1) into a reversed-phase high-performance preparative liquid chromatograph, elute isocratically, and detect online with an ultraviolet detector, and collect orlistat preparation components in a targeted ...

Embodiment 2

[0048] (1) Dissolving and filtering:

[0049] According to the ratio of orlistat crude product solid mass:solvent volume=15g:1L, orlistat crude product solid is dissolved with mobile phase, after dissolving, filter with 0.45 μ m organic microporous membrane, and the filtrate is used as the next step to prepare purified orlistat Raw material of lixistat.

[0050] The purity of the orlistat of the crude product used is 97% (HPLC area normalization method), and the maximum simple impurity is 0.45% (HPLC does not add the principal component self-contrast method of correction factor, Chinese Pharmacopoeia 2010 edition, P appendix 31),

[0051] Acetonitrile-water solution with a volume ratio of 80:20 was selected as the mobile phase.

[0052] (2) separation and purification:

[0053] Inject 2.5 L of the filtrate in step (1) into a reversed-phase high-efficiency preparative liquid chromatograph, elute isocratically, and detect online with an ultraviolet detector to collect orlistat...

Embodiment 3

[0058] (1) Dissolving and filtering:

[0059] According to the ratio of orlistat crude product solid mass:solvent volume=20g:1L, orlistat crude product solid is dissolved with mobile phase, after dissolving, filter with 0.45 μ m organic microporous membrane, and the filtrate is used as the next step to prepare purified orlistat Raw material of lixistat.

[0060] The purity of the orlistat of the crude product used is 98% (HPLC area normalization method), and the maximum simple impurity is 0.44% (HPLC does not add the principal component self-contrast method of correction factor, Chinese Pharmacopoeia 2010 edition, P appendix 31),

[0061] The mobile phase was ethanol-water solution with a volume ratio of 88:12.

[0062] (2) separation and purification:

[0063] Inject 2.5 L of the filtrate in step (1) into a reversed-phase high-efficiency preparative liquid chromatograph, elute isocratically, and detect online with an ultraviolet detector to collect orlistat preparation comp...

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Abstract

The invention belongs to the field of separation and purification and relates to a method for separating and purifying Orlistat by reverse-phase high-performance preparative liquid chromatography. The Orlistat prepared by using the method has purity of more than 99.6%, recovery rate of above 90% and the largest single impurity content of not more than 0.1%. The method has the advantages of simplicity in process operation, easiness in quality control and suitability for wide industrial scale application.

Description

technical field [0001] The invention belongs to the field of separation and purification, and relates to a method for separation and purification of chemical substances, in particular to a method for separation and purification of orlistat by reverse-phase high-efficiency liquid chromatography. Background technique [0002] Orlistat (Orlistat, Tetrahydrolipstat), chemical name N-formyl-L-leucine-(S)-1-{[(2S,3S)-3-hexyl-4-oxo-2-oxa Cyclobutyl]methyl}dodecyl ester ((S)-N-formyl leuine(S)-1-[[(2S,3S)-3-hexyl-4-oxo-2oxetanyl]methyl]dodecyl ester) , the CAS number is 96829-58-2, and the structural formula is as follows: [0003] [0004] Orlistat is a specific gastrointestinal lipase inhibitor that can reduce obesity-related risk factors and the incidence of other obesity-related diseases, including hypercholesterolemia, type II diabetes, impaired glucose tolerance, Hyperinsulinemia, high blood pressure, and can reduce the fat content in organs. It is indicated for the long...

Claims

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Application Information

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IPC IPC(8): C07D305/12B01D15/08
Inventor 赵志全李铁健郝大伟
Owner SHANDONG NEWTIME PHARMA
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