Determination of illicit drugs and their metabolites in human urine by liquid chromatography tandem mass spectrometry including relative ion intensity criterion.
A method, using 0.5 mL of urine, was developed for the simultaneous determination of ecgonine methyl ester, benzoylecgonine, morphine, codeine, 6-acetylmorphine, amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), methadone, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP), and d-lysergic acid diethylamide (LSD). The analysis was performed by liquid chromatography with tandem mass spectrometry, after solid-phase extraction in the presence of their deuterated analogues. Reversed-phase separation on an Atlantis dC18 column was achieved in 12.5 min, under gradient conditions. The method was fully validated, including linearity (1-2000 microg/L for ecgonine methyl ester, benzoylecgonine, 6-acetylmorphine, methamphetamine, MDMA, and EDDP; 2-2000 microg/L for morphine, codeine, MDA, and methadone; 2-1000 microg/L for amphetamine, and 0.2-100 microg/L for LSD; r(2)>0.99); recovery (>65%), within-day and between-day precision, and accuracy (CV and MRE<15%); limit of detection (0.1 microg/L for LSD, 0.5 microg/L for ecgonine methyl ester, benzoylecgonine, methamphetamine, MDMA, 6-monoacetylmorphine, and EDDP, and 1 microg/L for amphetamine, MDA, morphine, and methadone); quantitation (lowest level of the calibration curve); relative ion intensities, freeze-and-thaw stability, and matrix effect. The procedure showed to be sensitive and specific, and was applied to real cases and quality control samples from a quality control program.
Concheiro
Marta
M
University of Santiago de Compostela, Forensic Toxicology Service, Spain.
De Castro
Ana
A
Quintela
Oscar
O
Cruz
Angelines
A
López-Rivadulla
Manuel
M
D000662:Amphetamines / Q000652:urine; D002853:Chromatography, Liquid; D003042:Cocaine / Q000031:analogs & derivatives / Q000652:urine; D006801:Humans; D013287:Illicit Drugs / Q000652:urine*; D008238:Lysergic Acid Diethylamide / Q000652:urine; D008691:Methadone / Q000652:urine; D009020:Morphine / Q000652:urine; D011759:Pyrrolidines / Q000652:urine; D053719:Tandem Mass Spectrometry
D000662:Amphetamines; D013287:Illicit Drugs; D011759:Pyrrolidines; C005618:benzoylecgonine; D009020:Morphine; D008238:Lysergic Acid Diethylamide; D003042:Cocaine; D008691:Methadone; C034524:ecgonine methyl ester; C010724:2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine