Amara Babu Namburi L A, Koganti Kalyani, Palakeeti Babji, Srinivas Koduri S V, Rao Koya Prabhakara
New Generation Materials Lab (NGML), Department of Science and Humanities, Vignan's Foundation for Science, Technology and Research (VFSTR) (Deemed to be University), Vadlamudi, Guntur, Andhra Pradesh, India.
Department of Chemistry, National Institute of Technology, Warangal, Telangana, India.
Biomed Chromatogr. 2021 Oct;35(10):e5178. doi: 10.1002/bmc.5178. Epub 2021 Jun 2.
A new RP-HPLC method with a quick, sensitive and stable indication for the quantitative measurement of selexipag and its associated substances was developed and validated in the present study. In this new method, using the impurity-spiked solution, the chromatographic approach was optimized. Similarly, using the X-bridge phenyl column with isocratic elution of mobile phase containing acetonitrile and formic acid, selexipag and its impurities were separated. Recovery experiments obtained were satisfactory, and also the calibration graphs plotted for selexipag and its five impurities were found to be linear. The system validation parameters such as specificity, linearity, precision, accuracy and robustness were determined successfully. The obtained results indicated that the developed method was found to be useful for analyzing selexipag from its impurities. Further, using stress tests against acid, alkali, peroxide, reduction, thermal, hydrolysis and UV conditions, the present established method of HPLC was assessed and validated as per ICH Q2(R1) guidelines.
本研究开发并验证了一种用于定量测定司来帕格及其相关物质的快速、灵敏且稳定的反相高效液相色谱（RP-HPLC）新方法。在这种新方法中，使用加标杂质溶液对色谱方法进行了优化。同样，使用X-桥苯基色谱柱，以含有乙腈和甲酸的流动相进行等度洗脱，实现了司来帕格及其杂质的分离。回收率实验结果令人满意，并且绘制的司来帕格及其五种杂质的校准曲线呈线性。成功确定了特异性、线性、精密度、准确度和稳健性等系统验证参数。所得结果表明，所开发的方法可用于分析司来帕格及其杂质。此外，根据国际协调会议（ICH）Q2(R1)指南，通过对酸、碱、过氧化物、还原、热、水解和紫外线条件进行强制降解试验，对本建立的高效液相色谱法进行了评估和验证。
