化学
色谱法
蛋白质沉淀
分析物
电喷雾电离
药代动力学
串联质谱法
萃取(化学)
选择性反应监测
高效液相色谱法
质谱法
内科学
医学
作者
Shihong Liu,Jing-Min Shi,Junpei Fan,Jie Sun,Suhui Zhang,Yue Hu,Wei Li,Chunhua Wu,Xiuli Chang,Liming Tang,Zhijun Zhou
摘要
Abstract A precise, high‐throughput and sensitive ultra‐performance liquid chromatography–tandem mass spectrometry (UPLC‐MS/MS) method has been developed for the determination of fluorochloridone (FLC) in rat plasma. The extraction of analytes from plasma samples was carried out by protein precipitation procedure using acetonitrile prior to UPLC‐MS/MS analysis. Verapamil was proved as a proper internal standard (IS) among many candidates. The chromatographic separation based on UPLC was well optimized. Multiple reaction monitoring in positive electrospray ionization was used with the optimized MS transitions at: m / z 312.0 → 292.0 for FLC and m / z 456.4 → 165.2 for IS. This method was well validated with good linear response ( r 2 > 0.998) observed over the investigated range of 3–3000 ng/mL and with satisfactory stability. This method was also characterized with adequate intra‐ and inter‐day precision and accuracy (within 12%) in the quality control samples, and with high selectivity and less matrix effect observed. Total running time was only 1.5 min. This method has been successfully applied to a pilot FLC pharmacokinetic study after oral administration. Copyright © 2016 John Wiley & Sons, Ltd.
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