Simultaneous analysis of amphetamine, methamphetamine, and 3, 4-methylenedioxymethamphetamine (MDMA) in urine samples by solid-phase extraction, derivatization, and gas chromatography/mass spectrometry.
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.
Gan
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Department of Criminal Justice, University of Alabama, Birmingham.
Baugh
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Liu
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Walia
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D015104:3,4-Methylenedioxyamphetamine / Q000652:urine*; D000661:Amphetamine / Q000652:urine*; D002138:Calibration; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D008694:Methamphetamine / Q000652:urine*; D011237:Predictive Value of Tests; D015203:Reproducibility of Results
D008694:Methamphetamine; D015104:3,4-Methylenedioxyamphetamine; D000661:Amphetamine