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A method for separating optical isomers of statins

A technology for optical isomers and separation methods, which is applied in material separation, scientific instruments, analytical materials, etc., can solve problems such as separation difficulties, and achieve the effects of ensuring drug safety, simple operation, good peak shape and reproducibility

Active Publication Date: 2022-06-28
HUNAN JIUDIAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Because its active 2S / 4R configuration is very similar to the physical and chemical properties of its optical isomers, it is difficult to separate these substances

Method used

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  • A method for separating optical isomers of statins
  • A method for separating optical isomers of statins
  • A method for separating optical isomers of statins

Examples

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Embodiment 1

[0057] A method for separating optical isomers in statins, the method is to separate (4R-cis)-6-aldehyde-2,2-dimethyl-1,3-dioxane-4-acetic acid tertiary The active ingredient 2S / 4R configuration of butyl ester is separated from 2S / 4S configuration and 2R / 4R configuration, and the method used is gas chromatography. The instruments and reagents used are as follows:

[0058] Reagent: dichloromethane, grade: AR, manufacturer: Sinopharm Group.

[0059] Instruments: gas chromatograph, model 7890B, manufacturer Agilent; electronic analytical balance, model XS205DU, manufacturer: Mettler.

[0060] The gas chromatography conditions were as follows:

[0061] Chromatographic column: Rt-bDEXm (30m×0.25mm×0.25μm), inlet temperature: 200℃, FID detector temperature 200℃, flow rate: 1.0ml / min, injection volume: 1ul, split ratio: 10:1 , carrier gas: nitrogen, heating program: the initial temperature is 100 °C, then the temperature is increased to 150 °C at a speed of 1 °C / min, and the tempe...

Embodiment 2

[0075] A method for separating optical isomers in statins, the method is to separate (4R-cis)-6-aldehyde-2,2-dimethyl-1,3-dioxane-4-acetic acid tertiary The active ingredient 2S / 4R configuration of butyl ester is separated from 2S / 4S configuration and 2R / 4R configuration, and the method used is gas chromatography. The instruments and reagents used are as follows:

[0076] Reagent: dichloromethane, grade: AR, manufacturer: Sinopharm Group.

[0077] Instruments: gas chromatograph, model 7890B, manufacturer Agilent; electronic analytical balance, model XS205DU, manufacturer: Mettler.

[0078] The gas chromatography conditions were as follows:

[0079] Chromatographic column: Rt-bDEXm (30m×0.25mm×0.25μm), inlet temperature: 200℃, FID detector temperature 200℃, flow rate: 1.0ml / min, injection volume: 1ul, split ratio: 10:1 , carrier gas: nitrogen, heating program: the initial temperature is 95 °C, then the temperature is increased to 150 °C at a speed of 1 °C / min, and the temper...

Embodiment 3

[0093] A method for separating optical isomers in statins, the method is to separate (4R-cis)-6-aldehyde-2,2-dimethyl-1,3-dioxane-4-acetic acid tertiary The 2S / 4R configuration of the active ingredient of butyl ester was separated from the 2R / 4S configuration by gas chromatography. The instruments and reagents used are as follows:

[0094] Reagent: dichloromethane, grade: AR, manufacturer: Sinopharm Group.

[0095] Instruments: gas chromatograph, model 7890B, manufacturer Agilent; electronic analytical balance, model XS205DU, manufacturer: Mettler.

[0096] The gas chromatography conditions were as follows:

[0097] Chromatographic column: MEGA-DEX DMT Beta (30m×0.25mm×0.25μm), inlet temperature: 200℃, FID detector temperature 220℃, flow rate: 1.0ml / min, injection volume: 1ul, split ratio: 10 : 1, carrier gas: nitrogen, heating program: the initial temperature is 130 °C, then the temperature is increased to 150 °C at a rate of 1 °C / min, and maintained for 10 min.

[0098] ...

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Abstract

The invention discloses a method for separating optical isomers in statin drugs. Gas chromatography is used to effectively detect and separate the optical isomer impurities of the statin drugs. The method is simple to operate, and can effectively detect and separate statin starting materials with similar boiling points and similar polarity and its optical isomers, and the impurities are baseline separated from adjacent peaks, and the peak shape and reproducibility are good. It also effectively fills the gap in the detection of related substances in the quality standard of rosuvastatin calcium optical isomers, can provide technical reference for the quality control of rosuvastatin calcium raw materials, and ensures the safety of medication.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for separating optical isomers of statins. Background technique [0002] (4R-cis)-6-aldehyde-2,2-dimethyl-1,3-dioxane-4-acetic acid tert-butyl ester is the starting material of statins (such as rosuvastatin), There are 2 chiral centers in its structure, and there are four optical isomers in total, and its structure is shown in the following formula: [0003] [0004] In addition to the active 2S / 4R configuration, there are 2R / 4R configuration, 2S / 4S configuration, 2R / 4S configuration, [0005] Its structure is shown in the following table: [0006] [0007] Because its active 2S / 4R configuration is very similar to its physicochemical properties of its optical isomers, it is difficult to separate these substances. [0008] Chinese patent CN201810477427.9 discloses a method for simultaneously detecting statin side chains and isomer impurities. The steps include: 1) t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/68
CPCG01N30/06G01N30/68
Inventor 苏艳红何娟刘波
Owner HUNAN JIUDIAN PHARMA