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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 26, Number 7, October 2002,
pp. 401-405
Evaluation of a Solid-Phase Extraction Method for Benzoylecgonine
Urine Analysis in a High-Throughput Forensic Urine Drug-Testing Laboratory*
Peter R. Stout, Jay M. Gehlhausen†, Carl K.
Horn, and Kevin L. Klette‡
Navy Drug Screening Laboratory, Naval Air Station, H-2033, Jacksonville, Florida
32212
A novel extraction and derivatization procedure for the cocaine
metabolite benzoylecgonine (BZE) was developed and evaluated for use in a high-volume
forensic urine analysis laboratory. Extractions utilized a Speedisk 48™
positive pressure extraction manifold and polymer-based cation-exchange extraction
columns. Samples were derivatized by the addition of pentafluoropropionic anhydride
and pentafluoropropanol. All analyses were performed in selected ion monitoring
mode; ions included m/z 421, 300, 272, 429, and 303 with m/z 421 to 429 ratio
used for quantitation. The average extraction efficiency was 80%. Seventy-five
common over-the-counter products, including prescription drugs, drug metabolites,
and other drugs of abuse, demonstrated no significant interference with respect
to chromatography or quantitation. The limit of detection and limit of quantitation
were calculated at 12.5 ng/mL, and the assay was linear from 12.5 to 20,000
ng/mL with an r2 of 0.99932. A series of 20 precision samples (100 ng/mL) produced
an average response of 97.8 ng/mL and a percent coefficient of variation of
4.1%. A set of 79 archived human urine samples that had previously been found
to contain BZE were analyzed by 3 separate laboratories. The results did not
differ significantly from prior quantitation or between laboratories. The Speedisk
has proven viable for a high-volume production facility reducing overall cost
of analysis by decreasing analysis time and minimizing waste production while
meeting strict forensic requirements.
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