A validated method for the determination of nicotine, cotinine, trans-3'-hydroxycotinine, and norcotinine in human plasma using solid-phase extraction and liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry
A validated method for the determination of nicotine, cotinine, trans-3'-hydroxycotinine, and norcotinine in human plasma using solid-phase extraction and liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry
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DOI：
10.1002/jms.1039
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发表时间：
2006-06-01
影响因子：
2.3
通讯作者：
Huestis, Marilyn A.
中科院分区：
文献类型：
--
作者：
Kim, Insook;Huestis, Marilyn A.
开发并验证了同时测定人血浆中尼古丁、可替宁、反式-3-羟基可替宁和去甲可替宁的液相色谱-质谱法。使用固相萃取从人血浆中提取分析物和氘代内标物，并通过液相色谱/大气压化学电离-质谱检测和选择离子监测（SIM）进行分析。所有分析物的检测限和定量限分别为1.0和2.5 ng/ml。线性范围为2.5 - 500 ng/ml人血浆，加权因子为1/x;校准曲线的相关系数> 0.99。批内和批间精密度和准确度<15.0%。回收率为108.2-110.8%尼古丁、95.8-108.7%可替宁、90.5-99.5%反式-3 '-羟基可替宁和99.5-109.5%去甲可替宁。由于难以获得用于制备校准品和质量控制（QC）样品的无尼古丁人血浆，该方法还在牛血清中进行了部分验证。经证明，该方法对于在尼古丁对脑活动和母亲吸烟者新生儿发育的急性影响的临床研究中采集的人血浆中尼古丁、可替宁、反式-3 '-羟基可替宁和去甲可替宁的定量具有耐用性和准确度。版权所有（c）2006约翰威利父子有限公司。
A liquid chromatographic-mass spectrometric method for the simultaneous determination of nicotine, cotinine, trans-3-hydroxycotinine, and norcotinine in human plasma was developed and validated. Analytes and deuterated internal standards were extracted from human plasma using solid-phase extraction and analyzed by liquid chromatography/atmospheric pressure chemical ionization-mass spectrometric detection with selected ion monitoring (SIM). Limits of detection and quantification were 1.0 and 2.5 ng/ml, respectively, for all analytes. Linearity ranged from 2.5 to 500 ng/ml of human plasma using a weighting factor of 1/x; correlation coefficients for the calibration curves were > 0.99. Intra- and inter-assay precision and accuracy were < 15.0%. Recoveries were 108.2-110.8% nicotine, 95.8-108.7% cotinine, 90.5-99.5% trans-3'-hydroxycotinine, and 99.5-109.5% norcotinine. The method was also partially validated in bovine serum, owing to the difficulty of obtaining nicotine-free human plasma for the preparation of calibrators and quality control (QC) samples. This method proved to be robust and accurate for the quantification of nicotine, cotinine, trans-3'-hydroxycotinine, and norcotinine in human plasma collected in clinical studies of acute nicotine effects on brain activity and on the development of neonates of maternal smokers. Copyright (c) 2006 John Wiley & Sons, Ltd.