title: Automated determination of 'Ecstasy' and amphetamines in urine by SPME and capillary gas chromatography after propylchloroformate derivatisation.
abstract: The determination of amphetamines and their methylenedioxylated analogs in urine by propylchloroformate derivatisation and automated solid-phase microextraction is described. The urine sample was adjusted to pH 10.8 and added propylchloroformate reagent and an internal standard. Derivatisation resulted in water-stable carbamates which were automatically extracted by solid-phase microextraction. A fiber coated with polydimethylsiloxane was inserted into the urine matrix and agitated for 16 min. The fibre with the extracted carbamates was injected into the heated split-splitless injection port of the gas chromatograph where the analytes were evaporated at 300 degrees C, separated on a methylsilicone capillary column and detected by either a nitrogen phosphorous detector or by mass spectrometry. The method was shown to be highly reproducible and robust with respect to variations in the urine matrices. The detection limits were 5 ng/ml(-1) of methamphetamine, MDMA and MDEA and 15 ng/ml(-1) of amphetamine and MDA in urine. The method is a solvent free, automated alternative to traditional methods for determination of the amphetamine and their methylendioxylated analogs in urine.
authors.affiliation: Institute of Pharmacy, University of Oslo, Norway.
authors.forename: H G
authors.initials: HG
authors.lastname: Ugland
authors.forename: M
authors.initials: M
authors.lastname: Krogh
authors.forename: K E
authors.initials: KE
authors.lastname: Rasmussen
mesh_terms: D015104:3,4-Methylenedioxyamphetamine / Q000031:analogs & derivatives / Q000652:urine; D000662:Amphetamines / Q000652:urine*; D015198:Designer Drugs / Q000032:analysis*; D004952:Esters / Q000737:chemistry; D005069:Evaluation Studies as Topic; D005561:Formates / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D018817:N-Methyl-3,4-methylenedioxyamphetamine / Q000652:urine*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D015813:Substance Abuse Detection / Q000379:methods*
chemical_list: D000662:Amphetamines; D015198:Designer Drugs; D004952:Esters; D005561:Formates; D015104:3,4-Methylenedioxyamphetamine; D018817:N-Methyl-3,4-methylenedioxyamphetamine; C051800:3,4-methylenedioxyethamphetamine