Suresh P S, Mullangi Ramesh, Sukumaran Sathesh Kumar
Department of Pharmaceutics, School of Pharmaceutical Sciences, Vels Institute of Science Technology and Advanced Studies, Vels University, Chennai, 600117, India.
Biomed Chromatogr. 2014 Dec;28(12):1633-40. doi: 10.1002/bmc.3191. Epub 2014 May 7.
A rapid and highly sensitive assay method has been developed and validated for the estimation of galantamine (GLM) in rat plasma using liquid chromatography coupled to tandem mass spectrometry with electrospray ionization in the positive-ion mode. The assay procedure involves a simple liquid-liquid extraction of GLM and phenacetin (internal standard, IS) from rat plasma using acetonitrile. Chromatographic separation was achieved with 0.2% formic acid:acetonitrile (50:50, v/v) at a flow rate of 0.60 mL/min on an Atlantis dC18 column with a total run time 2.5 min. The MS/MS ion transitions monitored were 288.10 → 213.10 for GLM and 180.10 → 110.10 for IS. Method validation was performed as per United States Food and Drug Administration guidelines and the results met the acceptance criteria. The lower limit of quantitation achieved was 0.12 ng/mL and linearity was observed from 0.12 to 525 ng/mL. The intra- and inter-day precision were in the ranges of 4.73-11.7 and 5.83-8.64%, respectively. This novel method has been applied to a pharmacokinetic study in rats.
已开发并验证了一种快速且高度灵敏的测定方法，用于使用液相色谱-串联质谱联用技术（电喷雾电离正离子模式）测定大鼠血浆中的加兰他敏（GLM）。该测定程序包括使用乙腈从大鼠血浆中简单液-液萃取GLM和非那西丁（内标，IS）。在Atlantis dC18柱上，以0.2%甲酸：乙腈（50:50，v/v）为流动相，流速为0.60 mL/min，实现色谱分离，总运行时间为2.5分钟。监测的MS/MS离子跃迁对于GLM为288.10→213.10，对于IS为180.10→110.10。按照美国食品药品监督管理局的指南进行方法验证，结果符合验收标准。实现的定量下限为0.12 ng/mL，在0.12至525 ng/mL范围内观察到线性关系。日内和日间精密度分别在4.73 - 11.7%和5.83 - 8.64%范围内。这种新方法已应用于大鼠的药代动力学研究。
