title: Determination of paramethoxyamphetamine and other amphetamine-related designer drugs by liquid chromatography/sonic spray ionization mass spectrometry.
abstract: Paramethoxyamphetamine (PMA) is an amphetamine-like designer drug that has emerged recently on the European illicit drug market. This drug has a wicked reputation, as a number of lethal intoxications have occurred. A method using high-performance liquid chromatography coupled to ion trap based mass spectrometry (LC/MS) is described for the determination of this compound together with 3,4-methylenedioxymethamphetamine (XTC or MDMA), amphetamine and 3,4-methylenedioxyamphetamine (MDA) in human matrices. A liquid/liquid extraction (LLE) was applied to whole blood, urine and postmortem tissues. Reversed-phase liquid chromatography was performed on a narrow-bore phenyl-type column at a flow rate of 0.3 mL/min. A switch box allowed disposal of early-eluting irrelevant material to waste, protecting the mass spectrometer from contamination. The column effluent was directed into an ion trap mass spectrometer by a sonic spray ionization (SSI) interface. The method was validated for all three matrices, proving the applicability of SSI even when dealing with complex biological matrices. The within-and between-day precisions were less than 17.5% and accuracy was below 16.2%. Weighted (1/x) quadratic calibration curves were generated ranging from 10 to 1000 ng/mL (blood and urine) or 20 to 2000 ng/g (tissue) and correlation coefficients (r(2)) always exceeded 0.995. In addition, the mass spectrum of PMA is given together with a proposed fragmentation pattern for the obtained LC/MS spectrum. This information can be useful for future identification of PMA with LC/MS in biological matrices as well as in confiscated powders or tablets.
authors.affiliation: Laboratorium voor Toxicologie, Universiteit Gent, Harelbekestraat 72, B-9000 Gent, Belgium.
authors.forename: Kjell A
authors.initials: KA
authors.lastname: Mortier
authors.forename: Riet
authors.initials: R
authors.lastname: Dams
authors.forename: Willy E
authors.initials: WE
authors.lastname: Lambert
authors.forename: Els A
authors.initials: EA
authors.lastname: De Letter
authors.forename: Serge
authors.initials: S
authors.lastname: Van Calenbergh
authors.forename: André P
authors.initials: AP
authors.lastname: De Leenheer
mesh_terms: D015104:3,4-Methylenedioxyamphetamine / Q000031:analogs & derivatives* / Q000032:analysis; D000661:Amphetamine / Q000032:analysis*; D000662:Amphetamines; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D015198:Designer Drugs / Q000032:analysis*; D005554:Forensic Medicine / Q000379:methods*; D006801:Humans; D018817:N-Methyl-3,4-methylenedioxyamphetamine / Q000032:analysis; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
chemical_list: D000662:Amphetamines; D015198:Designer Drugs; C016575:3,4-methylenedioxyphenethylamine; D015104:3,4-Methylenedioxyamphetamine; D000661:Amphetamine; D018817:N-Methyl-3,4-methylenedioxyamphetamine; C100230:4-methoxyamphetamine