Automated determination of ‘Ecstasy’ and amphetamines in urine by SPME and capillary gas chromatography after propylchloroformate derivatisation

• Published in: Journal of pharmaceutical and biomedical analysis 1999-03, Vol.19 (3), p.463-475
• Main Authors: Grefslie Ugland, Hege, Krogh, Mette, Rasmussen, Knut E
• Format: Article
• Language: English
• Subjects: 3,4-Methylenedioxyamphetamine - analogs & derivatives; 3,4-Methylenedioxyamphetamine - urine; Amphetamines; Amphetamines - urine; Analysis; Aqueous derivatisation; Biological and medical sciences; Designer Drugs - analysis; Drug addictions; Ecstasy; Esters - chemistry; Evaluation Studies as Topic; Formates - chemistry; Gas chromatography; Gas Chromatography-Mass Spectrometry; General pharmacology; Humans; Medical sciences; N-Methyl-3,4-methylenedioxyamphetamine - urine; Pharmacology. Drug treatments; Reproducibility of Results; Sensitivity and Specificity; SPME; Substance Abuse Detection - methods; Toxicology
• ISSN: 0731-7085; 1873-264X
• DOI: 10.1016/S0731-7085(98)00240-4

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°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.