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建立并验证了一种 EI-GC/MS 方法,用于测定血液中的舍曲林及其主要代谢物去甲舍曲林。

Development and validation of an EI-GC/MS method for the determination of sertraline and its major metabolite desmethyl-sertraline in blood.

机构信息

Department of Forensic Medicine and Toxicology, School of Medicine, National and Kapodistrian University of Athens, 75 Mikras Asias, Athens 115 27, Greece.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Sep 1;879(25):2576-82. doi: 10.1016/j.jchromb.2011.07.015. Epub 2011 Jul 20.

DOI:10.1016/j.jchromb.2011.07.015
PMID:21813341
Abstract

A sensitive and specific GC/MS method for the determination of sertraline and its main metabolite desmethyl-sertraline in whole blood has been developed, optimized and validated. Sample preparation included solid-phase extraction of both analytes and their derivatization with heptafluorobutyric anhydride (HFBA). Protriptyline was used as internal standard for the determination of both analytes. Limits of detection and quantification for both sertraline and desmethyl-sertraline were 0.30 and 1.00 μg/L, respectively. The calibration curves were linear within the dynamic range of each analyte (1.00-500.0 μg/L) with a correlation coefficient (R(2)) exceeding 0.991. Extraction efficiency ranged from 90.1(± 5.8)% to 95.4(± 3.0)% for sertraline, and from 84.9(± 8.2)% to 107.7(± 4.4)% for desmethyl-sertraline. The precision for sertraline and desmethyl-sertraline was between 3.6-5.5% and 4.7-7.2%, respectively, while the accuracy was in the range of -6.67% to 2.20% and -6.33% to 2.88% for sertraline and desmethyl-sertraline, respectively. The method was applied to real blood samples obtained from patients that follow sertraline treatment and also in cases of forensic interest. The developed method can be used in routine every day analysis by clinical and forensic laboratories, for pharmacokinetic studies, for therapeutic sertraline monitoring or for the investigation of forensic cases where sertraline is involved.

摘要

已经开发、优化和验证了一种用于测定全血中舍曲林及其主要代谢物去甲舍曲林的灵敏、特异的 GC/MS 方法。样品制备包括两种分析物的固相萃取及其与七氟丁酰酐(HFBA)的衍生化。普罗替林被用作两种分析物的内标。舍曲林和去甲舍曲林的检测限和定量限分别为 0.30 和 1.00 μg/L。校准曲线在每个分析物的动态范围内均呈线性(1.00-500.0 μg/L),相关系数(R²)均超过 0.991。舍曲林的提取效率范围为 90.1(±5.8)%至 95.4(±3.0)%,去甲舍曲林的提取效率范围为 84.9(±8.2)%至 107.7(±4.4)%。舍曲林和去甲舍曲林的精密度分别在 3.6-5.5%和 4.7-7.2%之间,而准确度分别在-6.67%至 2.20%和-6.33%至 2.88%之间。该方法应用于接受舍曲林治疗的患者的真实血液样本以及法医学感兴趣的情况下。开发的方法可用于临床和法医实验室的常规日常分析、药代动力学研究、治疗性舍曲林监测或涉及舍曲林的法医案例调查。

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