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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 31, Number 9, November/December,
pp.573-580
Determination of Illicit Drugs and their
Metabolites in Human Urine by Liquid Chromatography Tandem
Mass Spectrometry Including Relative Ion Intensity Criterion
Marta Concheiro, Ana De Castro, Oscar
Quintela, Angelines Cruz, and Manuel López-Rivadulla
University of Santiago de Compostela, Forensic Toxicology
Service, Spain
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 µg/L
for ecgonine methyl ester, benzoylecgonine, 6-acetylmorphine,
methamphetamine, MDMA, and EDDP; 2–2000 µg/L for
morphine, codeine, MDA, and methadone; 2–1000 µg/L
for amphetamine, and 0.2–100 µg/L for LSD; r2 > 0.99);
recovery (> 65%), within-day and between-day precision, and
accuracy (CV and MRE < 15%); limit of detection (0.1 µg/L
for LSD, 0.5 µg/L for ecgonine methyl ester, benzoylecgonine,
methamphetamine, MDMA, 6-monoacetylmorphine, and EDDP, and 1 µg/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.
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