Simultaneous Analysis of Amphetamine, Methamphetamine, and 3,4-Methylenedioxymethamphetamine (MDMA) in Urine Samples by Solid-Phase Extraction, Derivatization, and Gas Chromatography/Mass Spectrometry

A solid-phase extraction method using Bond Elute Certify™ cartridges extracts amphetamine, methamphetamine, and MDMA from urine. The extract is derivatized with trichloroacetic anhydride and analyzed by gas chromatography/mass spectrometry with selected ion monitoring. Recovery exceeds 65% with less than 5% coefficient of variation. The lowest detectable concentration is about 50 ng/mL using a 2 mL sample. Within the 250 to 4000 ng/mL range, a second-order polynomial model yields a near-perfect fit.

Study at a glance

Abstract

Abstract A rapid and effective solid-phase extraction procedure using Bond Elute Certify™ bonded silica sorbent cartridges was adopted to extract amphetamine, methamphetamine, and 3,4-methylenedioxymethamphetamine (MDMA or Ecstasy) from urine samples. The extract was derivatized with trichloroacetic anhydride prior to gas chromatography/mass spectrometry (GC/MS) analysis with selected ion monitoring of the following ions: 190, 91, 188; 204, 91, 202; 162, 135, 202; 194, 123; and 211, 209 for the derivatized amphetamine, methamphetamine, MDMA, d5-amphetamine, and d9-methamphetamine, respectively. The first of the ions listed for each compound was used for quantitation. The compound d5-amphetamine was used as the internal standard for amphetamine, and d9-methamphetamine was used for methamphetamine and MDMA. Results showed a higher than 65% recovery and a reproducibility with less than a 5% coefficient of variation. When a sample size of 2 mL was used, the lowest detectable concentration was about 50 ng/mL, and a near-perfect fit can be obtained (within the 250 to 4000-ng/mL concentration range studied) using a second-order polynomial model.