Forensic Toxicology and Chemistry Laboratory, Criminalistics Institute of São Paulo, Sao Paulo, SP, Brazil; Institute of Chemistry, University of Sao Paulo, Sao Paulo, SP, Brazil.
Institute of Legal Medicine, Sao Paulo State Police, Sao Paulo, Brazil.
J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Jan 15;945-946:84-91. doi: 10.1016/j.jchromb.2013.10.014. Epub 2013 Oct 21.
This work presents the development of an analytical method based on capillary electrophoresis with diode array detection for the analysis of drugs of abuse and biotransformation products in vitreous humor. Composition of the background electrolyte, implementation of an online pre-concentration strategy and sample preparation procedures were objects of study. The complete electrophoretic separation of 12 analytes (amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyethylamphetamine (MDEA), ketamine, cocaine, cocaethylene, lidocaine, morphine, 6-monoacetylmorphine and heroin) and the internal standard N-methyl-1-(3,4-methylenedioxyphenyl)-2-butamine (MBDB) was obtained within 13min of run. The method was validated presenting good linearity (r(2)>0.99), recovery ≥90%, precision better than 12% RSD and acceptable accuracy in the range of 86-118% at three concentration levels (50, 100 and 500ng/mL). LODs and LOQs in the order of 1-5ng/mL and 5-10ng/mL, respectively, were obtained. After validation, the method was applied to eighty-seven vitreous humor samples and the results were compared to those obtained by a liquid chromatography tandem mass spectrometry (LC-MS/MS) screening method, routinely used by the forensic toxicology laboratory of the Sao Paulo State Police, Brazil. Cocaine was detected in 7.1%, cocaethylene in 3.6%, lidocaine in 2.4% and ketamine in 1.2% of the total number of analyzed samples.
本工作开发了一种基于毛细管电泳-二极管阵列检测的分析方法，用于检测玻璃体液中的滥用药物和生物转化产物。研究了背景电解质的组成、在线浓缩策略的实施和样品制备程序。在 13 分钟的运行时间内，实现了 12 种分析物（苯丙胺、甲基苯丙胺、3,4-亚甲二氧基苯丙胺（MDA）、3,4-亚甲二氧基甲基苯丙胺（MDMA）、3,4-亚甲二氧基乙基苯丙胺（MDEA）、氯胺酮、可卡因、可乐因、利多卡因、吗啡、6-单乙酰吗啡和海洛因）和内标 N-甲基-1-（3,4-亚甲二氧基苯基）-2-丁胺（MBDB）的完全电泳分离。该方法具有良好的线性（r(2)>0.99）、回收率≥90%、精密度优于 12%RSD 和在三个浓度水平（50、100 和 500ng/mL）范围内的可接受准确性。LODs 和 LOQs 分别为 1-5ng/mL 和 5-10ng/mL。方法验证后，应用于 87 例玻璃体液样本，并将结果与巴西圣保罗州警察法医毒理学实验室常规使用的液相色谱串联质谱（LC-MS/MS）筛选方法进行比较。可卡因在 7.1%的总分析样本中检出，可乐因在 3.6%的总分析样本中检出，利多卡因在 2.4%的总分析样本中检出，氯胺酮在 1.2%的总分析样本中检出。
