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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 26, Number 3, April,
pp. 253-261
Rapid Simultaneous Determination of Amphetamine, Methamphetamine,
3,4-Methylenedioxyamphetamine, 3,4-Methylenedioxymethamphetamine, and 3,4-Methylenedioxyethylamphetamine
in Urine by Solid-Phase Extraction and GC–MS: A Method Optimized for High-Volume
Laboratories
Peter R. Stout, Carl K. Horn, and Kevin L. Klette
Navy Drug Screening Laboratory, P.O. Box 113, Bldg. H-2033, Naval Air Station,
Jacksonville, Florida 32212
To facilitate analysis of
high sample volumes, an extraction, derivatization and gas chromatographic–mass
spectrometric analysis method was developed to simultaneously determine amphetamine
(AMP), methamphetamine (MAMP), 3,4-methylenedioxyamphetamine (MDA) 3,4-methylenedioxymethamphetamine
(MDMA), and 3,4-methylenedioxyethylamphetamine (MDEA) in urine. This method
utilized a positive-pressure manifold cation-exchange polymer-based solid-phase
extraction followed by elution directly into automated liquid sampler (ALS)
vials. Rapid derivatization was accomplished using heptafluorobutyric anhydride
(HFBA). Recoveries averaged 90% or greater for each of the compounds. Limits
of detection were 62.5 ng/mL (AMP and MDEA), 15.6 ng/mL (MAMP), and 31.3 ng/mL
(MDA and MDMA) using a 2-mL sample volume. The method was linear to 5000 ng/mL
for all compounds using MDMA-d5 and MAMP-d14 as internal standards. Over 200
human urine samples previously determined to contain the target analytes were
analyzed using the method. Excellent agreement was seen with previous quantitations.
The method was challenged with 75 potentially interfering compounds and no interferences
were seen. These interfering compounds included ephedrine, pseudoephedrine,
phenylpropanolamine, and phenethylamine. The method resulted in dramatic reductions
in processing time and waste production. Reproduction
of editorial content of this journal is prohibited without publisher’s
permission.
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