PMID- 21147046 OWN - NLM STAT- MEDLINE DCOM- 20110411 LR - 20191210 IS - 1873-376X (Electronic) IS - 1570-0232 (Linking) VI - 879 IP - 1 DP - 2011 Jan 1 TI - Stereoselective method development and validation for determination of concentrations of amphetamine-type stimulants and metabolites in human urine using a simultaneous extraction-chiral derivatization approach. PG - 8-16 LID - 10.1016/j.jchromb.2010.10.037 [doi] AB - Amphetamine-type stimulants (ATS) are a group of chiral amine drugs which are commonly abused for their sympathomimetic and stimulant properties. ATS are extensively metabolised by hepatic cytochrome P450 enzymes. As metabolism of ATS has been shown to be highly stereospecific, stereoselective analytical methods are essential for the quantitative determination of ATS concentrations for both in vivo and in vitro studies of ATS metabolism. This paper describes a new stereoselective method for the simultaneous determination of amphetamine (AM), methamphetamine (MA), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), 4-hydroxy-3-methoxymethamphetamine (HMMA), 4-hydroxy-3-methoxyamphetamine (HMA), 3,4-hydroxymethamphetamine (HHMA) and 3,4-hydroxyamphetamine (HHA) in human urine samples validated according to the United States Food and Drug Administration guidelines. In this method, analytes are simultaneously extracted and derivatized with R-(-)-alpha-methoxy-alpha-(trifluoromethyl)phenylacetyl chloride (R-MTPCl) as the chiral derivatization reagent. Following this, the analytes were subjected to a second derivatization with N-methyl-N-trimethylsilyltrifluoroacetamide (MSTFA) which targets the hydroxyl groups present in HMMA, HMA, HHMA and HHA. The derivatized analytes were separated and quantified using gas chromatography-mass spectrometry (GC-MS). The method was evaluated according to the established guidelines for specificity, linearity, precision, accuracy, recovery and stability using a five-day protocol. Intra-day precision ranged from 0.89 to 11.23% RSD whereas inter-day precision was between 1.03 and 12.95% RSD. Accuracy values for the analytes ranged from -5.29% to 13.75%. Limits of quantitation were 10 mug/L for AM, MA, MDMA, HMA and HMMA and 2mug/L for MDA, HMA and HHA. Recoveries and stability values were also within accepted values. The method was applied to authentic ATS-positive samples. CI - Crown Copyright (c) 2010. Published by Elsevier B.V. All rights reserved. FAU - Wan Raihana, W A AU - Wan Raihana WA AD - Department of Pharmacology, School of Medical Sciences, Universiti Sains Malaysia, 16150 Kubang Kerian, Kelantan, Malaysia. FAU - Gan, S H AU - Gan SH FAU - Tan, S C AU - Tan SC LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20101124 PL - Netherlands TA - J Chromatogr B Analyt Technol Biomed Life Sci JT - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JID - 101139554 RN - 0 (Amphetamines) RN - 0 (Illicit Drugs) SB - IM MH - Amphetamines/chemistry/isolation & purification/*urine MH - Chemical Fractionation/*methods MH - Drug Stability MH - Drug Users MH - Gas Chromatography-Mass Spectrometry/*methods MH - Humans MH - Illicit Drugs/chemistry/isolation & purification/*urine MH - Least-Squares Analysis MH - Reproducibility of Results MH - Sensitivity and Specificity MH - Stereoisomerism EDAT- 2010/12/15 06:00 MHDA- 2011/04/13 06:00 CRDT- 2010/12/15 06:00 PHST- 2010/08/25 00:00 [received] PHST- 2010/10/27 00:00 [revised] PHST- 2010/10/28 00:00 [accepted] PHST- 2010/12/15 06:00 [entrez] PHST- 2010/12/15 06:00 [pubmed] PHST- 2011/04/13 06:00 [medline] AID - S1570-0232(10)00684-7 [pii] AID - 10.1016/j.jchromb.2010.10.037 [doi] PST - ppublish SO - J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Jan 1;879(1):8-16. doi: 10.1016/j.jchromb.2010.10.037. Epub 2010 Nov 24.