Published: Journal of Analytical Toxicology, ISSN 0146-4760, Volume 30, Number 8, October 2006, pp.559-562

Validation of a Headspace GC Method for the Analysis of a Pyrolytic Product of Methamphetamine in Urine
Diaa M. Shakleya[1], James C. Kraner[2], David J. Clay[2], Patrick S. Callery[3], and Suzanne C. Bell[1]
[1]Chemistry Department, West Virginia University, Morgantown, West Virginia;
[2]Office of the Chief Medical Examiner, Charleston, West Virginia; and
[3]Basic Pharmaceutical Sciences, West Virginia University, Morgantown, West Virginia

A method has been developed and validated using headspace GC–FID for the identification of 1-phenylpropene in urine. This compound is a pyrolytic product of methamphetamine that has been previously proposed as a marker for smoked methamphetamine. The instrumentation used is the same as employed for blood alcohol determination. The extraction-free procedure is rapid, simple, and quantitative using 2-phenylpropene as the internal standard. The method was validated for linearity over a range of 0.1–20 µg/mL with a limit of detection of 0.05 µg/mL, limit of quantification of 0.1 µg/mL, interday accuracy within 3.2 to –5.3%, intraday accuracy better than 7.5%, interday precision of 7.5 to 10.7%, intraday precision of 2 to 8.6%, and recovery above 80%. For the robustness determination in urine, the accuracy of four different sources of urine at the mid control level (1 µg/mL) ranged from 1.6 to 19% error. The % relative standard deviation of the different urine sources ranged from 3.1 to 11%. Urine samples from nine methamphetamine-positive cases investigated by the Office of the Chief Medical Examiner of West Virginia were included in the study. 1-Phenylpropene was found in two methamphetamine-positive cases (0.25 and 0.44 µg/mL).

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