Ponnayyan Sulochana Suresh, Ravichandiran Vishnuvardh, Mullangi Ramesh, Sukumaran Sathesh Kumar
Department of Pharmaceutics, School of Pharmaceutical Sciences, Vels Institute of Science Technology and Advanced Studies (VISTAS), Vels University, Chennai 600117, India.
Jubilant Biosys Ltd, Industrial Suburb, Yeshwanthpur, Bangalore 560 022, India.
J Chromatogr Sci. 2016 Mar;54(3):397-404. doi: 10.1093/chromsci/bmv155. Epub 2015 Nov 10.
A rapid and highly sensitive assay method has been developed and validated for the estimation of tacrine 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 tacrine and phenacetin (internal standard, IS) from rat plasma using ethyl acetate. Chromatographic separation was achieved with 0.2% formic acid : acetonitrile (30 : 70, v/v) at a flow rate of 0.50 mL/min on an Atlantis dC18 column with a total run time of 3.0 min. The MS-MS ion transitions monitored were 199.10 → 171.20 for tacrine and 180.10 → 110.10 for IS. Method validation was performed as per United States Food and Drug Administration (US FDA) guidelines and the results met the acceptance criteria. The lower limit of quantification achieved was 0.008 ng/mL and linearity was observed from 0.008 to 53.4 ng/mL. The intra- and inter-day precision was in the range of 2.76-12.5 and 5.15-12.8%, 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，用于采用液相色谱-串联质谱联用（电喷雾电离，正离子模式）测定大鼠血浆中的他克林。该测定程序包括使用乙酸乙酯从大鼠血浆中简单液-液萃取他克林和非那西丁（内标，IS）。在Atlantis dC18柱上，以0.2%甲酸:乙腈（30:70，v/v）为流动相，流速为0.50 mL/min，总运行时间为3.0 min，实现色谱分离。监测的MS-MS离子跃迁对于他克林为199.10→171.20，对于内标为180.10→110.10。按照美国食品药品监督管理局（US FDA）指南进行方法验证，结果符合验收标准。实现的定量下限为0.008 ng/mL，在0.008至53.4 ng/mL范围内观察到线性关系。日内和日间精密度分别在2.76 - 12.5%和5.15 - 12.8%范围内。这种新方法已应用于大鼠的药代动力学研究。
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