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新型基于选择性的法医毒理学验证:全血中八种苯丙胺类兴奋剂的纸喷雾质谱定量检测方法。

Novel Selectivity-Based Forensic Toxicological Validation of a Paper Spray Mass Spectrometry Method for the Quantitative Determination of Eight Amphetamines in Whole Blood.

机构信息

ThoMSon Mass Spectrometry Laboratory, University of Campinas - UNICAMP, Campinas, 13083-970, Brazil.

Department of Chemistry and Center for Analytical Instrumentation, Purdue University, West Lafayette, IN, 47907, USA.

出版信息

J Am Soc Mass Spectrom. 2017 Dec;28(12):2665-2676. doi: 10.1007/s13361-017-1790-0. Epub 2017 Sep 6.

Abstract

Paper spray tandem mass spectrometry is used to identify and quantify eight individual amphetamines in whole blood in 1.3 min. The method has been optimized and fully validated according to forensic toxicology guidelines, for the quantification of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxy-N-methylamphetamine (MDMA), 3,4-methylenedioxy-N-ethylamphetamine (MDEA), para-methoxyamphetamine (PMA), para-methoxymethamphetamine (PMMA), and 4-fluoroamphetamine (4-FA). Additionally, a new concept of intrinsic and application-based selectivity is discussed, featuring increased confidence in the power to discriminate the amphetamines from other chemically similar compounds when applying an ambient mass spectrometric method without chromatographic separation. Accuracy was within ±15% and average precision was better than 15%, and better than 20% at the LLOQ. Detection limits between 15 and 50 ng/mL were obtained using only 12 μL of whole blood. Graphical abstract ᅟ.

摘要

纸喷雾串联质谱法用于在 1.3 分钟内鉴定和定量全血中的八种个体苯丙胺。该方法已根据法医毒理学指南进行了优化和全面验证,用于定量检测苯丙胺、甲基苯丙胺、3,4-亚甲二氧基苯丙胺 (MDA)、3,4-亚甲二氧基-N-甲基苯丙胺 (MDMA)、3,4-亚甲二氧基-N-乙基苯丙胺 (MDEA)、对甲氧基苯丙胺 (PMA)、对甲氧基苯丙胺 (PMMA) 和 4-氟苯丙胺 (4-FA)。此外,还讨论了一种新的固有和基于应用的选择性概念,其特点是在应用无需色谱分离的环境质谱方法时,增加了从其他化学相似化合物中区分苯丙胺的能力的可信度。准确度在 ±15% 以内,平均精密度优于 15%,在LLOQ 时优于 20%。使用仅 12 μL 的全血即可获得 15 至 50ng/mL 的检测限。

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