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

Ber K. Gan, Daniel Baugh, Rh Liu, As Walia

Journal of Forensic Sciences September 1, 1991 DOI: 10.1520/jfs13155j (opens in new tab)

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AI-extracted from the abstract
Characteristics Method development and validation Peer reviewed
Population Urine samples
Topics MDMA
Keywords Methamphetamine Derivatization Solid phase extraction Gas chromatography–mass spectrometry Selected ion monitoring Elution Extraction chemistry Urine Pharmacology
Citations 54
Key points The solid-phase extraction and GC/MS method achieves over 65% recovery, less than 5% variation, and a detection limit of about 50 ng/mL for amphetamine, methamphetamine, and MDMA in urine.

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.

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