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采用填充固相微萃取和气相色谱-串联质谱法测定人血浆中的七种选定的抗精神病药物。

Determination of seven selected antipsychotic drugs in human plasma using microextraction in packed sorbent and gas chromatography-tandem mass spectrometry.

机构信息

CICS-UBI-Centro de Investigação em Ciências da Saúde, Universidade da Beira Interior, Covilhã, Portugal.

出版信息

Anal Bioanal Chem. 2013 May;405(12):3953-63. doi: 10.1007/s00216-012-6695-y. Epub 2013 Jan 12.

DOI:10.1007/s00216-012-6695-y
PMID:23314486
Abstract

A method using microextraction by packed sorbent (MEPS) and gas chromatography-tandem mass spectrometry (GC-MS/MS) is described for the determination of seven antipsychotic drugs in human plasma. The studied compounds were chlorpromazine (CPZ), haloperidol (HAL), cyamemazine, quetiapine, clozapine, olanzapine (OLZ), and levomepromazine; promazine, protriptyline, and deuterated CPZ were used as internal standards. The validation parameters included selectivity, linearity and limits of detection and quantitation, intra- and interday precision and trueness, recovery, and stability and were studied according to internationally accepted guidelines. The method was found to be linear between the lower limit of quantitation and 1000 ng/mL, except for OLZ and HAL (200 ng/mL), with determination coefficients higher than 0.99 for all analytes, and extraction efficiencies ranged from 62 to 92 %. Intra- and interday precision ranged from 0.24 to 10.67 %, while trueness was within a ±15 % interval from the nominal concentration for all analytes at all studied levels. MEPS has shown to be a rapid procedure for the determination of the selected antipsychotic drugs in human plasma, allowing reducing the handling time and the costs of analysis. Furthermore, GC-MS/MS has demonstrated to be a powerful tool for the simultaneous quantitation of the studied compounds, enabling obtaining adequate selectivity and sensitivity using a sample volume of as low as 0.25 mL.

摘要

一种使用填充固相微萃取(MEPS)和气相色谱-串联质谱(GC-MS/MS)的方法被用于测定人血浆中的七种抗精神病药物。所研究的化合物包括氯丙嗪(CPZ)、氟哌啶醇(HAL)、氰美嗪、喹硫平、氯氮平、奥氮平(OLZ)和左美丙嗪;奋乃静、普罗替林和氘代 CPZ 被用作内标。验证参数包括选择性、线性和检测限和定量限、日内和日间精密度和准确度、回收率以及稳定性,并根据国际公认的指南进行了研究。该方法在定量下限和 1000ng/mL 之间呈线性,除 OLZ 和 HAL(200ng/mL)外,所有分析物的决定系数均高于 0.99,萃取效率在 62%至 92%之间。日内和日间精密度在 0.24%至 10.67%之间,而准确度在所有研究水平下均在名义浓度的±15%范围内。MEPS 已被证明是一种快速测定人血浆中所选抗精神病药物的方法,可以减少处理时间和分析成本。此外,GC-MS/MS 已被证明是同时定量研究化合物的有力工具,仅使用 0.25mL 样品体积即可获得足够的选择性和灵敏度。

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