Liu Ji, Zhou Xiao
Department of Anesthesia, Shanghai Pulmonary Hospital, Tongji University School of Medicine.
J Chromatogr Sci. 2013 Jan;51(1):59-64. doi: 10.1093/chromsci/bms106. Epub 2012 Jun 21.
The objective of this work was to develop a simple, cost effective, rugged and rapid method for the simultaneous estimation of zolmitriptan (ZP) and its active metabolite n-desmethy-zolmitriptan (DZP) in rat plasma to meet the requirement for biological sample analysis. The simple liquid-liquid extraction employed in the present work gave consistent and reproducible recoveries for both the analytes. A mixture of methanol-20 mM ammonium acetate-formic acid (60:40:0.1, v/v/v) was used as mobile phase at a flow rate of 0.3 mL/min. The temperature of column and autosampler were maintained at 40 and 4°C, respectively. The chromatographic run time of each sample was 3.0 min. The limit of quantification was low enough to monitor at least four half-lives of ZP and DZP concentrations with good intra-assay and inter-assay reproducibility for the quality controls. According to the results of all the validation parameters, the method can also be useful for pharmacokinetics study of ZP and for therapeutic drug monitoring in humans with the desired precision and accuracy.
本研究的目的是开发一种简单、经济高效、耐用且快速的方法,用于同时测定大鼠血浆中的佐米曲普坦(ZP)及其活性代谢物N-去甲基佐米曲普坦(DZP),以满足生物样品分析的要求。本研究采用的简单液-液萃取法对两种分析物均能给出一致且可重复的回收率。以甲醇-20 mM醋酸铵-甲酸(60:40:0.1,v/v/v)的混合物作为流动相,流速为0.3 mL/min。柱温箱和自动进样器的温度分别保持在40°C和4°C。每个样品的色谱运行时间为3.0分钟。定量限足够低,能够监测ZP和DZP浓度的至少四个半衰期,且质量控制的批内和批间重现性良好。根据所有验证参数的结果,该方法对于ZP的药代动力学研究以及人类治疗药物监测也具有所需的精密度和准确度。