Authors: Klette, Kevin; Jamerson, Matthew H.; Morris-Kukoski, Cynthia L.; Kettle, Aaron R.; Snyder, J. Jacob J.

Source: Journal of Analytical Toxicology, Volume 29, Number 7, October 2005 , pp. 669-674(6)

Publisher: Preston Publications

Abstract:

The use of fast gas chromatography–mass spectrometry (FGC–MS) was investigated to improve the efficiency of analysis of urine specimens that previously screened presumptively positive for amphetamine (AMP), methamphetamine (MAMP), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), and/or 3,4 methylenedioxyethylamphetamine (MDEA) by immunoassay testing. Specimens were pretreated with basic sodium periodate, extracted using a positive-pressure manifold/cation-exchange solid-phase cartridge methodology, and derivatized using 4-carbethoxyhexafluorobutyryl chloride (4-CB). The analytical method was compared to traditional GC–MS analysis and evaluated with respect to assay chromatography, linearity, sensitivity, precision, accuracy, and reproducibility. The limits of detection were 62.5 ng/mL for MDA and 31.25 ng/mL for AMP, MAMP, MDMA, and MDEA. All of the target analytes were linear to 12,000 ng/mL with the exception of MAMP which was linear to 10,000 ng/mL. The intra-assay precision of a 500 ng/mL multi-constituent control (n = 15) ranged from 522.6 to 575.9 ng/mL with a coefficient of variation of less than 3.8%. Authentic human urine specimens (n =187) previously determined to contain the target analytes were re-extracted and analyzed by both FGC–MS and the currently utilized GC–MS method. No significant differences in specimen concentration were observed between these analytical methods. No interferences were seen when the performance of the FGC–MS method was challenged with ephedrine, pseudoephedrine, phenylpropanolamine, and phentermine. When compared to traditional GC–MS analysis, FGC–MS analysis provided a dramatic reduction in retention time for amphetamine (1.8 min vs. 4.12 min). For example, the FGC–MS method reduced overall run time for a batch of 56 specimens from 12.0 h to 7.25 h. This reduction in analysis time makes FGC–MS an attractive alternative to traditional GC–MS by allowing a laboratory greater flexibility in the purchase and use of capital equipment and in the assignment of laboratory personnel, all resulting in greater overall efficiency by decreasing reporting times for AMP, MAMP, and designer amphetamine positive specimens.

Document Type: Research article

Affiliations: 1: Navy Drug Screening Laboratory, 320B B Street, Great Lakes, Illinois 60088-2815

Publication date: 2005-10-01

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• The Journal of Analytical Toxicology (JAT), established in 1977 and published 9 times a year, is the international source covering a broad range of clinical, forensic, and industrial laboratory topics regarding the isolation, identification, and quantitation of potentially toxic substances.

  With an emphasis on practical application, JAT articles provide improved and novel techniques for use in clinical, forensic, workplace, sports testing (doping), and other toxicology laboratories. Articles describe newly developed methods in immunoassay testing, gas chromatography, liquid chromatography, mass spectrometry, atomic absorption spectrometry, solid and liquid phase extraction techniques, and other analytical approaches. Worldwide readership includes toxicologists, pathologists, chemists, clinicians, researchers, and educators working in medical examiner and law enforcement laboratories, hospitals, university and independent analytical laboratories, as well as the drug manufacturing industry.

  Each year in October, we publish a special issue from the Society of Forensic Toxicologists.

  JAT, as determined by ISI Citation Index, is one of the two most referenced international journals in forensic science.

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