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气相色谱-质谱联用仪在溶剂中添加甲酸测定血清中的异戊巴比妥和苯巴比妥

Determination of amobarbital and phenobarbital in serum by gas chromatography-mass spectrometry with addition of formic acid to the solvent.

作者信息

Saka Kanju, Uemura Koichi, Shintani-Ishida Kaori, Yoshida Ken-ichi

机构信息

Department of Forensic Medicine, Graduate School of Medicine, University of Tokyo, Tokyo, Japan.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Jun 15;869(1-2):9-15. doi: 10.1016/j.jchromb.2008.05.004. Epub 2008 May 10.

Abstract

A rapid and accurate method for quantification of amobarbital and phenobarbital was developed using gas chromatography-mass spectrometry (GC-MS) without derivatization. Though the compounds measured without derivatization showed low sensitivity because of adsorption, addition of 3% formic acid to the solvent improved the sensitivity for the analytes. Taking account of matrix effect, solid-phase and liquid-liquid extraction from serum were examined. The correlation coefficients of the calibration curves were 0.9995 or better, and the accuracy and precision of intraday and interday assays were in line with Food and Drug Administration (FDA) criteria.

摘要

建立了一种无需衍生化的气相色谱-质谱联用(GC-MS)法,用于快速、准确地定量异戊巴比妥和苯巴比妥。尽管未经衍生化测定的化合物因吸附作用而灵敏度较低,但向溶剂中添加3%的甲酸可提高分析物的灵敏度。考虑到基质效应,对血清的固相萃取和液液萃取进行了研究。校准曲线的相关系数为0.9995或更高,日内和日间测定的准确度和精密度均符合美国食品药品监督管理局(FDA)的标准。

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