Determination of 19 drugs of abuse and metabolites in whole blood by high-performance liquid chromatography–tandem mass spectrometry

摘要: A high-performance liquid chromatography (LC)–tandem mass spectrometry (MS/MS) method has been developed and validated for the determination of 19 drugs abuse metabolites used in whole blood. The following compounds were included: amphetamine, methylenedioxyamphetamine, methylenedioxyethylamphetamine, methylenedioxymethamphetamine, methamphetamine, cocaine, benzoylecgonine, morphine, 6-acetylmorphine, codeine, methadone, buprenorphine, norbuprenorphine, ketobemidone, tramadol, O-desmethyltramadol, zaleplone, zolpidem, zopiclone. sample pretreatment consisted solid-phase extraction using mixed-mode columns (Isolute Confirm HCX). Deuterated analogues as internal standards all analytes, except ketobemidone O-desmethyltramadol. analytes separated by a methanol/ammonium formate gradient LC (Agilent HPLC 1100) with 3 mm × 100 mm Varian Pursuit 3 C18 column, 3-µm particle size, quantified MS/MS (Waters Quattro micro tandem quadrupole spectrometer) multiple reaction monitoring positive mode. Two transitions tramadol run time was 35 min including equilibration time. For responses linear over range investigated, R 2 > 0.99. One-point calibration found to be adequate validation, thereby saving analysis calibrators. limits quantification (LOQs) ranged from 0.0005 0.01 mg/kg. Absolute recoveries 34 97%, zaleplone (6%). Both interday precision intraday less than 15% (20% at LOQ) norburprenorphine, (less 18%). Accuracy (bias) within ±15% (±20% MDMA O-desmethyltramadol (within ±19%). No ion suppression or enhancement seen nor coeluted seen. Matrix effects 23% zopiclone (64%). High-concentration low-concentration quality control samples gave acceptable values, tried international proficiency test schemes good results. present LC-MS/MS provides simple, specific, sensitive solution some most frequent their successfully applied 412 forensic cases October 2008 mid February 2009, where 267 related zero-tolerance traffic legislation.