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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 30, Number 8, October 2006,
pp.554-558
Rapid Analysis of Benzoylecgonine in Urine by Fast Gas
Chromatography–Mass Spectrometry
Robert W. Romberg, Matthew H. Jamerson, and Kevin L. Klette
Navy Drug Screening Laboratory, 320B B Street, Great Lakes, Illinois 60088-2815
A novel fast gas chromatography–mass spectrometry (FGC–MS)
analytical method for benzoylecgonine (BZE) has been developed to improve the
efficiency of specimen analysis without diminishing the reliability of metabolite
identification and quantification. Urine specimens were spiked with deuterated
internal standard (BZE-d8), subjected to solid-phase extraction, and derivatized
with pentafluoropropionic anhydride (PFPA) and pentafluoropropanol (PFPOH).
The pentafluoropropyl ester derivative of BZE was identified and quantified
using both a standard GC–MS method and the newly developed FGC–MS
method. Shorter GC analyte retention times were made possible in the FGC–MS
method by employing a 220-volt GC oven controller, which allowed an increased
temperature ramp rate. The FGC–MS method was linear between 25 and 10,000
ng/mL of BZE yielding a correlation coefficient of 0.9994. The intra-assay precision
of a 100 ng/mL BZE standard (n = 15) yielded an average concentration of 99.7
ng/mL and a coefficient of variation of 1.2%. The interassay precision of 21
sets of 50, 100, and 125 ng/mL BZE controls was found to be acceptable, with
coefficients of variation less than 2.4%. No interference was observed when
the FGC–MS method was challenged with cocaine, ecgonine, ecgonine methyl
ester, and nine other drugs of abuse. Analysis of presumptively positive specimens
(n = 146) by both analytical methods yielded comparable results with a correlation
coefficient of 0.996. The FGC–MS method, when compared with a standard
GC–MS method, reduces total assay time by approximately 50% while demonstrating
comparable reliability.
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