Separation determination method of rivaroxaban optical isomer

A technology for optical isomers and rivaroxaban, which is applied in the field of separation and determination of optical isomers of rivaroxaban, can solve the problems of losing chiral recognition ability and destroying spatial structure, achieving good separation and accurate results , the effect of high sensitivity

Inactive Publication Date: 2013-07-24
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the coated chiral column uses organic solvents such as tetrahydrofuran, methyl tert-butyl ether, and chlorinated reagents as the mobile phase, the chiral stationary phase will be partially or completely swollen or dissolved, destroying the spatial structure and losing chirality recognition ability

Method used

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  • Separation determination method of rivaroxaban optical isomer
  • Separation determination method of rivaroxaban optical isomer
  • Separation determination method of rivaroxaban optical isomer

Examples

Experimental program
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Effect test

Embodiment 1

[0032] A method for separating and measuring optical isomers of rivaroxaban, specifically comprising the steps of:

[0033] (1) Chromatographic separation of optical isomers of rivaroxaban

[0034] Weigh 10 mg of the rivaroxaban sample (S configuration) to be tested, use a 10 ml volumetric flask to set the volume to the mark, shake well, and use it as the test solution 1, the injection flow rate is 1.0 ml / min, and the detection wavelength is 250 nm; Select an IC chiral chromatographic column, the column temperature is 30°C, the injection volume is 5 μl, the mobile phase is acetonitrile=100%, and the flow rate of the mobile phase is set to 0.7ml / min to complete the separation of the optical isomers of rivaroxaban to be tested;

[0035] (2) Determination of the content of optical isomers of rivaroxaban

[0036] Weigh about 10 mg of rivaroxaban racemate standard sample, dissolve it with acetonitrile, use a 10 ml volumetric flask to adjust the volume to the mark, shake well, and ...

Embodiment 2

[0043] Take the test solution 2 obtained in Example 1 respectively, and according to the chromatographic conditions, the detection wavelength: 250nm, column temperature: 30°C, flow rate: 0.7ml / min; mobile phase: acetonitrile-water=40-60 (V / V) Carry out chromatographic analysis, record the chromatogram, see the results figure 2 ;

[0044] figure 2 The chromatographic peak at 31.562min is the chromatographic peak of rivaroxaban in S configuration, and the chromatographic peak at 27.688min is the chromatographic peak of rivaroxaban in R configuration in the optical isomer of rivaroxaban.

[0045] The chromatogram of the obtained rivaroxaban optical isomer sample (S configuration) was compared with the separation chromatogram of the rivaroxaban racemate standard sample obtained in step (2) of Example 1 by using the area normalization method , so that the content of rivaroxaban in S configuration in the optical isomers of rivaroxaban to be tested is 38%, and the content of rivaro...

Embodiment 3

[0048] Take the test solution 2 obtained in Example 1 respectively, and according to the chromatographic conditions, the detection wavelength: 250nm, column temperature: 30°C, flow rate: 0.7ml / min; mobile phase: acetonitrile-water=90-10 (V / V) Carry out chromatographic analysis, record the chromatogram, see the results image 3 ;

[0049] image 3 The chromatographic peak at 9.547min is the chromatographic peak of rivaroxaban in S configuration, and the chromatographic peak at 8.877min is the chromatographic peak of rivaroxaban in R configuration, which is the optical isomer of rivaroxaban.

[0050] The chromatogram of the obtained rivaroxaban optical isomer sample (S configuration) was compared with the separation chromatogram of the rivaroxaban racemate standard sample obtained in step (2) of Example 1 by using the area normalization method , so that the content of rivaroxaban in S configuration in the optical isomers of rivaroxaban to be tested is 38%, and the content of r...

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Abstract

The invention relates to a separation determination method of a rivaroxaban optical isomer. According to the invention, proper amounts of a rivaroxaban optical isomer sample requiring detection and a rivaroxaban racemate standard sample with known component contents are fetched, and are respectively dissolved by using acetonitrile, such that acetonitrile solutions of the rivaroxaban optical isomer sample requiring detection and of the rivaroxaban racemate standard sample with known component contents are prepared; a bonded chiral column CHIRALPAKIC column is adopted, and feeding is carried out; a detection wavelength is 210-260nm, a column temperature is 15-35 DEG C, a feeding volume is 5-20mul, and a mobile phase flow rate is controlled at 0.7-1.0ml/min, such that the separation of the rivaroxaban optical isomer requiring separation is finished; and with an area normalization method, the obtained separation spectrum of the rivaroxaban optical isomer sample requiring detection and the separation spectrum of the rivaroxaban racemate standard sample with known component contents are compared, such that S-configuration and R-configuration rivaroxaban contents in the rivaroxaban optical isomer requiring detection are calculated.

Description

technical field [0001] The invention relates to a method for separating and measuring optical isomers of rivaroxaban, in particular to a method for separating and measuring optical isomers of rivaroxaban by using high performance liquid chromatography. Background technique [0002] Rivaroxaban (Rivaroxaban) is a new oral anticoagulant drug that is highly selective and competitive and directly inhibits the free state of factor Xa, and can also inhibit the binding state of factor Xa and prothrombin activity. Has no direct effect on platelet aggregation. It has the characteristics of high bioavailability, broad disease spectrum for treatment, stable dose-effect relationship, convenient oral administration and low bleeding risk. Rivaroxaban (rivaroxaban, BAY5927939, trade name: Xarelto) chemical name: 5-chloro-N-{[2-oxo-3-[4-(3-oxomorpholin-4-yl)phenyl] Oxazolidinone-5-yl]methyl}thiophene-2-carboxamide, its chemical structural formula is as follows: [0003] The optical isom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 闫茜潘仙华许旭
Owner SHANGHAI INST OF TECH
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