Bévalot Fabien, Bottinelli Charline, Cartiser Nathalie, Fanton Laurent, Guitton Jérôme
1 Laboratoire LAT LUMTOX, 71 Avenue Rockefeller, Lyon 69003, France.
J Anal Toxicol. 2014 Jun;38(5):256-64. doi: 10.1093/jat/bku029. Epub 2014 Apr 30.
An automated solid-phase extraction (SPE) protocol followed by gas chromatography coupled with tandem mass spectrometry was developed for quantification of caffeine, cyamemazine, meprobamate, morphine and 6-monoacetylmorphine (6-MAM) in 11 biological matrices [blood, urine, bile, vitreous humor, liver, kidney, lung and skeletal muscle, brain, adipose tissue and bone marrow (BM)]. The assay was validated for linearity, within- and between-day precision and accuracy, limits of quantification, selectivity, extraction recovery (ER), sample dilution and autosampler stability on BM. For the other matrices, partial validation was performed (limits of quantification, linearity, within-day precision, accuracy, selectivity and ER). The lower limits of quantification were 12.5 ng/mL(ng/g) for 6-MAM, morphine and cyamemazine, 100 ng/mL(ng/g) for meprobamate and 50 ng/mL(ng/g) for caffeine. Analysis of real-case samples demonstrated the performance of the assay in forensic toxicology to investigate challenging cases in which, for example, blood is not available or in which analysis in alternative matrices could be relevant. The SPE protocol was also assessed as an extraction procedure that could target other relevant analytes of interest. The extraction procedure was applied to 12 molecules of forensic interest with various physicochemical properties (alimemazine, alprazolam, amitriptyline, citalopram, cocaine, diazepam, levomepromazine, nordazepam, tramadol, venlafaxine, pentobarbital and phenobarbital). All drugs were able to be detected at therapeutic concentrations in blood and in the alternate matrices.
开发了一种自动化固相萃取(SPE)方案,随后采用气相色谱-串联质谱法,用于定量分析11种生物基质[血液、尿液、胆汁、玻璃体液、肝脏、肾脏、肺和骨骼肌、脑、脂肪组织和骨髓(BM)]中的咖啡因、氰美马嗪、甲丙氨酯、吗啡和6-单乙酰吗啡(6-MAM)。该检测方法在BM上进行了线性、日内和日间精密度与准确度、定量限、选择性、提取回收率(ER)、样品稀释和自动进样器稳定性的验证。对于其他基质,进行了部分验证(定量限、线性、日内精密度、准确度、选择性和ER)。6-MAM、吗啡和氰美马嗪的定量下限为12.5 ng/mL(ng/g),甲丙氨酯为100 ng/mL(ng/g),咖啡因为50 ng/mL(ng/g)。实际案例样本分析证明了该检测方法在法医毒理学中用于调查具有挑战性的案例的性能,例如在无法获得血液或分析替代基质可能相关的案例中。SPE方案也被评估为一种可以针对其他相关感兴趣分析物的提取程序。该提取程序应用于12种具有不同理化性质的法医感兴趣分子(阿利马嗪、阿普唑仑、阿米替林、西酞普兰、可卡因、地西泮、左美丙嗪、去甲西泮、曲马多、文拉法辛、戊巴比妥和苯巴比妥)。所有药物在血液和替代基质中的治疗浓度下均能被检测到。