Screening procedure for 21 amphetamine-related compounds in urine using solid-phase microextraction and gas chromatography-mass spectrometry

Journal of Chromatographic Science
C BattuG Lachâtre

Abstract

A specific, sensitive, and rapid procedure for the screening of 21 amphetamine-related compounds in urine is developed using solid-phase microextraction (SPME) and gas chromatography-mass spectrometry. Very clean extracts are obtained in one step with SPME using silica fibers coated with a 100-micron polydimethylsiloxane stationary phase. Temperature, time, pH, and salt saturation are optimized to obtain consistent extraction. An excellent chromatographic separation of the underivatized analytes is obtained with a specially treated nonpolar capillary column (Supelco PTA-5, 30 m x 0.32-mm i.d., 0.5-micron film thickness) dedicated to amino compounds. Selected ion monitoring of three fragments per analyte and one for each of the three deuterated internal standards elicits a high selectivity and detection limits between 1 and 50 ng/mL (i.e., low enough to verify positive results obtained with immunochemical assays). The method is linear in a narrow range (from the detection limit up to 500 ng/mL) when all the amphetamines are assayed together but shows a good linearity up to 2000 ng/mL when the molecules are determined individually. Repeatability is not satisfactory for all compounds but could probably be improved by strictly cont...Continue Reading

Citations

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