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

• NCJ Number: 132512
• Journal: Journal of Forensic Sciences Volume: 36 Issue: 5 Dated: (September 1991) Pages: 1331-1341
• Author(s): B K Gan; D Baugh; R H Liu; A S Walia
• Date Published: 1991
• Length: 11 pages
• Publication Format: Article
• Publication Type: Test/Measurement
• Language: English
• Country: United States of America

Annotation

Using Bond Elute Certify, solid-phase extraction methodology was applied to the isolation and concentration of drug amphetamines from urine samples.

Abstract

The recovery process included column manufacturer extraction procedures, trichloroacetic anhydride derivatization, and the addition of a simple cleanup step prior to the derivatization. Gas chromatographic/mass spectrometric analysis was performed 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 (AMP), methamphetamine (MAP), 3,4- methylenedioxymethamphetamine (MDMA), d5-AMP, and d9-MAP, respectively. The first of the ions listed for each compound was used for quantitation. Using d5AMP as the internal standard, the recovery was 66, 81, and 97 percent for AMP, METH, and MDMA, respectively. With d9-MAP as the internal standard, the corresponding values were 66, 81, and 95 percent. Reproducibility was less than a 5- percent coefficient of variation. Analysis of a sample size of 2 milliters provided a detection limit of 50 nanograms/milliliter within a calibration range of 250 to 4000 ng/ml using a second order polynomial model. These data indicate this solid phase extraction method is effective for routine and high-volume testing of amphetamine drugs. 6 figures, 3 tables, and 8 references (Author abstract modified)