Negative-ion chemical ionization gas chromatography-mass spectrometry assay for enantioselective measurement of amphetamines in oral fluid: Application to a controlled study with MDMA and driving under the influence cases
Negative-ion chemical ionization gas chromatography-mass spectrometry assay for enantioselective measurement of amphetamines in oral fluid: Application to a controlled study with MDMA and driving under the influence cases
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DOI：
10.1373/clinchem.2006.081547
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发表时间：
2007-04-01
影响因子：
9.3
通讯作者：
Maurer, Hans H.
中科院分区：
文献类型：
--
作者：
Peters, Frank T.;Samyn, Nele;Maurer, Hans H.
背景资料：苯丙胺（AM）、甲基苯丙胺（MA）、3，4-亚甲二氧基苯丙胺（MDA）、3，4-亚甲二氧基甲基苯丙胺（MDMA）和3，4-亚甲二氧基乙基苯丙胺（MDEA）的对映选择性分析有助于解释毒理学结果。方法已被描述为各种矩阵，但到目前为止暴乱的口腔液，矩阵的重要性越来越大，在测试药物滥用，特别是在驾驶的药物的影响下（DUID）的背景下，方法：稀释后，用200 μ L碳酸盐缓冲液（pH 9），口腔液样品（10-50 μ L）进行衍生化与S-七氟丁酰脯氨酰氯。所得非对映异构体。提取到100 μ L环己烷中，通过气相色谱法（HP-5 MS柱）分离，并通过质谱法在负离子化学电离模式（GC-NICI-MS）下检测。该方法进行了验证，并适用于从一个对照研究与MDMA和正宗DUID cases.Results：衍生AM，MA，MDA，MDMA，MDEA对映体的样品，以及彼此分离。该方法在5-250 μ g/L MDA每种对映体和25-1250 μ g/L AM、MA、MDMA和MDEA每种对映体范围内呈线性。除MDEA外，分析回收率、重复性和中间精密度均在要求限度内。分析物的浓度和对映异构体的比例在应用程序中的样品相关性只有弱与相应的公布的血浆data.Conclusions：这种灵敏，可靠，快速的GC-NICI-MS分析antienoselectively措施AM，MA，MDA，和MDMA在口腔液样品。从各自的口腔液数据预测血浆浓度和对映体比率是不可能的。(c)2007年美国临床化学协会。
Background: Enantioselective analysis of amphetamine (AM), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethaitphetamine (MDMA), and 3,4-methylenedioxyethylamphetamine (MDEA) helps interpret toxicological results. Methods have been described for various matrices, but so far riot for oral fluid, a matrix of increasing importance in testing for drugs of abuse, especially in the context of driving under the influence of drugs (DUID).Methods: After dilution with 200 mu L carbonate buffer (pH 9), oral fluid samples (10-50 mu L) were derivatized with S-heptafluorobutyrylprolyl chloride. The resulting diastereomers. were extracted into 100 mu L of cyclohexane, separated by gas chromatography (HP-5MS column), and detected by mass spectrometry in the negative-ion chemical ionization mode (GC-NICI-MS). The method was validated and applied to samples from a controlled study with MDMA and from authentic DUID cases.Results: The derivatized AM, MA, MDA, MDMA, and MDEA enantiomers were well separated from each other. The method was linear from 5-250 mu g/L per enantiomer of MDA and from 25-1250 mu g/L per enantiomer of AM, MA, MDMA, and MDEA. With the exception of MDEA, analytical recoveries, repeatability, and intermediate precision were within required limits. The analyte concentrations and enantiomer ratios in the application samples correlated only weakly with corresponding published plasma data.Conclusions: This sensitive, reliable, and fast GC-NICI-MS assay enantioselectively measures AM, MA, MDA, and MDMA in oral fluid samples. Prediction of plasma concentrations And enantiomer ratios from respective oral fluid data is riot possible. (c) 2007 American Association for Clinical Chemistry.