PMID- 18262381 OWN - NLM STAT- MEDLINE DCOM- 20080729 LR - 20080512 IS - 0731-7085 (Print) IS - 0731-7085 (Linking) VI - 47 IP - 2 DP - 2008 Jun 9 TI - Liquid chromatography-atmospheric pressure ionization electrospray mass spectrometry determination of "hallucinogenic designer drugs" in urine of consumers. PG - 335-42 LID - 10.1016/j.jpba.2007.12.039 [doi] AB - A procedure based on liquid chromatography-mass spectrometry (LC-MS) is described for determination of 3,4-methylenedioxymethamphetamine (MDMA), 2,5-dimethoxy-4-methyl-phenethylamine (2C-D), 4-bromo-2,5-dimethoxy-beta-phenethylamine (2C-B), 1-(8-bromo-2,3,6,7-tetrahydrobenzo[1,2-b:4,5-b'] difuran-4-yl)-2-aminoethane (2C-B-Fly), 4-ethylthio-2,5-dimethoxy-beta-phenethylamine (2C-T-2), 4-iodo-2,5-dimethoxy-beta-phenethylamine (2C-I), and 4-ethyl-2,5-dimethoxy-beta-phenethylamine (2C-E), 1-(m-chlorophenyl)piperazine (m-CPP), 4-hydroxy-N,N-diisopropyltryptamine (4-OH-DIPT) and 4-acetoxy-N,N-diisopropyltryptamine (4-acetoxy-DIPT) in urine of consumers using 3,4 methylendioxypropylamphetamine (MDPA) as internal standard. Sample preparation involved a solid-phase extraction procedure at pH 6 of both non-hydrolyzed and enzymatically hydrolyzed urine samples. Chromatography was performed on a C(18) reversed-phase column using a linear gradient of 10mM ammonium bicarbonate, pH 7.3 and acetonitrile as a mobile phase. Separated analytes were determined in LC-MS single ion monitoring mode using an atmospheric pressure ionization-electrospray ionization (ESI) interface. The assay was tested on urine samples from consumers of compounds under investigation (n=32). Limits of quantification varied between 20 and 60 ng/mL for the different analytes under investigation. Calibration curves were linear to 2000 ng/mL for all the substances under investigation, with a minimum r(2)>0.99. At three concentrations spanning the linear dynamic range of the assay, mean recoveries ranged between 55.4 and 95.6% for the different analytes. Higher analytes concentrations in hydrolyzed samples showed the presence of conjugated compounds in urine. FAU - Pichini, Simona AU - Pichini S AD - Department of Therapeutic Research and Medicines Evaluation, Istituto Superiore di Sanita, Rome, Italy. simona.pichini@iss.it FAU - Pujadas, Mitona AU - Pujadas M FAU - Marchei, Emilia AU - Marchei E FAU - Pellegrini, Manuela AU - Pellegrini M FAU - Fiz, Jimena AU - Fiz J FAU - Pacifici, Roberta AU - Pacifici R FAU - Zuccaro, Piergiorgio AU - Zuccaro P FAU - Farre, Magi AU - Farre M FAU - de la Torre, Rafael AU - de la Torre R LA - eng PT - Comparative Study PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20080104 PL - England TA - J Pharm Biomed Anal JT - Journal of pharmaceutical and biomedical analysis JID - 8309336 RN - 0 (Designer Drugs) RN - 0 (Hallucinogens) SB - IM MH - Adult MH - *Atmospheric Pressure MH - Calibration MH - Chromatography, Liquid/*methods MH - Designer Drugs/*analysis/chemistry MH - Drug Stability MH - Female MH - Freezing MH - Hallucinogens/*analysis/urine MH - Humans MH - Male MH - Middle Aged MH - Reference Standards MH - Reproducibility of Results MH - Sensitivity and Specificity MH - Spectrometry, Mass, Electrospray Ionization/*methods MH - Substance Abuse Detection/*methods MH - Time Factors EDAT- 2008/02/12 09:00 MHDA- 2008/07/30 09:00 CRDT- 2008/02/12 09:00 PHST- 2007/10/09 00:00 [received] PHST- 2007/12/20 00:00 [revised] PHST- 2007/12/21 00:00 [accepted] PHST- 2008/02/12 09:00 [pubmed] PHST- 2008/07/30 09:00 [medline] PHST- 2008/02/12 09:00 [entrez] AID - S0731-7085(08)00003-4 [pii] AID - 10.1016/j.jpba.2007.12.039 [doi] PST - ppublish SO - J Pharm Biomed Anal. 2008 Jun 9;47(2):335-42. doi: 10.1016/j.jpba.2007.12.039. Epub 2008 Jan 4.