高效液相色谱法测定阿哌沙班异构体的建立与验证

IF 7.6 2区工程技术 Q1 CHEMISTRY, APPLIED

Annual review of chemical and biomolecular engineering Pub Date : 2020-01-04 DOI:10.11648/J.CBE.20200501.11

A. Gosar, R. Phadke, Deepesh Patil, K. Gupta, P. Thakur

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引用次数: 1

摘要

本研究旨在建立一种新颖、简便、精确、准确、经济的测定阿哌沙班原料药异构体含量的方法。阿哌沙班原料药有三种异构体:邻位异构体、间位异构体和对位异构体。在反相色谱法和正相色谱法中，这些异构体很难分离;因此采用了新的手性技术。采用chiralpak IA色谱柱(250×4.6×5µm)，采用等临界技术建立色谱方法。在波长290nm处检测异构体杂质。该方法按照ICH指南进行验证，回归分析显示阿哌沙班原料药及其异构体杂质的R值(相关系数)> 0.999。阿哌沙班在二氯甲烷中的溶液在48小时内稳定。降解研究是在ICH规定的指导方针内进行的。对该方法进行了线性度、准确度和精密度验证。

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Development and Validation of an New High Performance Liquid Chromatography Method for Determination of Apixaban Isomers

The purpose of this research study is to develop a novel, simple, precise, accurate and economical method for determination of Apixaban API isomers. Apixaban API has three isomer as ortho, meta and para. In reverse phase and normal phase chromatography it was very difficult to separate these isomer; hence new chiral technique was adopted. This chromatographic method was developed on chiralpak IA column (250×4.6×5µm) with isocritic technique. The detection of isomeric impurities were observed at wavelength 290nm. This analytical method was validated as per ICH guideline and regression analysis showed R value (correlation coefficient) > 0.999 for Apixaban API and its isomeric impurities. A solution of Apixaban in dichloromethane was found stable up to 48 hrs. The degradation study was done within the given guidelines prescribed by ICH. The method is validated for Linearity, Accuracy and Precision.

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来源期刊

Annual review of chemical and biomolecular engineering CHEMISTRY, APPLIED-ENGINEERING, CHEMICAL

CiteScore

16.00

自引率

0.00%

发文量

期刊介绍： The Annual Review of Chemical and Biomolecular Engineering aims to provide a perspective on the broad field of chemical (and related) engineering. The journal draws from disciplines as diverse as biology, physics, and engineering, with development of chemical products and processes as the unifying theme.