Rapid Analysis of Four Amphetamines in Urine by Self-Made Pipette-Tip Solid-Phase Extraction Followed by GC-MS/MS

A simple and rapid pipette-tip solid-phase extraction (PT-SPE) procedure with derivatization prior to gas chromatography triple quadrupole mass spectrometry analysis is developed for the simultaneous determination of amphetamine (AMP), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA) and 3,4-methylenedioxymethamphetamine (MDMA) in urine samples. The PT-SPE procedure using self-made sorbent could extract drugs within 6 min from 100-μL urine samples, requiring low solvent-consumption (<2.0 mL). Besides, the self-made pipette tip could be reused at least five times. Under optimized conditions, the recoveries of four amphetamines at spiked levels (low, medium and high) ranged from 87.7 to 110.4%, with relative standard deviations < 9.5%. The limit of detections and limit of quantifications for AMP, MA, MDA and MDMA were in the range of 2.52-8.25 ng⋅mL-1 and 8.4-27.5 ng⋅mL-1, respectively. Validation results show that the proposed method is suitable for the quantitation of amphetamines and has been successfully applied in the urine samples of suspected drug abusers.