RESUMO
A forensic procedure for the quantitative confirmation of lysergic acid diethylamide (LSD) and the qualitative confirmation of its metabolite, N-demethyl-LSD, in blood, serum, plasma, and urine samples is presented. The Zymark RapidTrace was used to perform fully automated solid-phase extractions of all specimen types. After extract evaporation, confirmations were performed using liquid chromatography (LC) followed by positive electrospray ionization (ESI+) mass spectrometry/mass spectrometry (MS/MS) without derivatization. Quantitation of LSD was accomplished using LSD-d3 as an internal standard. The limit of quantitation (LOQ) for LSD was 0.05 ng/mL. The limit of detection (LOD) for both LSD and N-demethyl-LSD was 0.025 ng/mL. The recovery of LSD was greater than 95% at levels of 0.1 ng/mL and 2.0 ng/mL. For LSD at 1.0 ng/mL, the within-run and between-run (different day) relative standard deviation (RSD) was 2.2% and 4.4%, respectively.
Assuntos
Líquidos Corporais/química , Medicina Legal/instrumentação , Alucinógenos/análise , Dietilamida do Ácido Lisérgico/análogos & derivados , Dietilamida do Ácido Lisérgico/análise , Detecção do Abuso de Substâncias/instrumentação , Cromatografia Líquida de Alta Pressão , Medicina Legal/métodos , Cromatografia Gasosa-Espectrometria de Massas/métodos , Alucinógenos/isolamento & purificação , Humanos , Dietilamida do Ácido Lisérgico/isolamento & purificação , Manejo de Espécimes/métodos , Detecção do Abuso de Substâncias/métodosRESUMO
A method is described for the simultaneous analysis of 14 non-steroidal anti-inflammatory drugs (NSAIDS) in human serum using negative electrospray ionization-tandem mass spectrometry (ESI-MS/MS). After addition of internal standard and protein precipitation using acetonitrile, samples were transferred to autosampler vials for direct analysis without chromatography. Injection of an air bubble with the sample and a multiple reaction monitoring (MRM) method using argon collision-induced dissociation (CID) of analyte (M-H)- ions permitted integration of the product ion peak areas to produce reproducible quantitative data over the range of concentrations expected in serum during routine use of these drugs. The method permitted the analysis of 30 samples per hour. Two hundred fifty consecutive analyses did not adversely affect instrument sensitivity.
Assuntos
Anti-Inflamatórios não Esteroides/sangue , Proteínas Sanguíneas/isolamento & purificação , Cromatografia Líquida de Alta Pressão , Eletroforese Capilar , Humanos , Espectrometria de MassasRESUMO
The Zymark RapidTrace automated solid-phase extraction system has been evaluated for use in the urine drug-testing laboratory. Methods for cocaine metabolite (benzoylecgonine) and opiates (codeine and morphine) are described and evaluated. The linearity, precision, accuracy, recovery, and carryover statistics of these analytical protocols are presented. The advantages of extraction using the RapidTrace instead of solid-phase extraction with the manual vacuum manifold or liquid-liquid extraction methods are described.