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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 31, Number 8, October,
pp.515-521
Direct-Injection Mass Spectrometric Method
for the Rapid Identification of Fentanyl and Norfentanyl in
Postmortem Urine of Six Drug-Overdose Cases
Cody J. Peer[1], Diaa M. Shakleya[2],
Islam R. Younis[1], James C. Kraner[3], and Patrick S. Callery[1],
[1]Department of Basic Pharmaceutical Sciences, West Virginia
University, Morgantown, West Virginia 26506;
[2]Intramural Research
Program, National Institute on Drug Abuse, Baltimore, Maryland
21224; and
[3]Office of the Chief Medical Examiner, Charleston,
West Virginia 25302
A rapid mass spectrometric method was developed
for the identification of fentanyl and its major hepatic metabolite
norfentanyl in postmortem urine of six drug-overdose victims
involving fentanyl use. To reduce matrix effects or ion suppression,
sample preparation consisted of centrifugation and solid-phase
extraction. Deuterium-labeled internal standards (2H5-fentanyl
and 2H5-norfentanyl) were used to compensate for instrument variation
in signal, analyte recovery during sample preparation, and ion
suppression. Structural information for fentanyl and norfentanyl
were collected using mass spectrometry (MS) with electrospray
ionization (ESI) operated in the positive ion mode. Fentanyl
(m/z 337) was found in each of the six overdose cases by the
appearance of the MS–MS daughter ion on both an ion trap
and a triple-quadrupole MS resulting from the fragmentation pathway
of fentanyl (m/z 337 → 188). Norfentanyl was detected in
all six cases by the appearance of the MH+ ion, m/z 233, with
a single-quadrupole MS and confirmed in an ion trap MS. Ion suppression,
as determined by the comparison of ion intensities from spiked
samples in water with postmortem urine from the cases, ranged
from 18% to 98% in three ESI sources. The use of stable isotope-labeled
internal standards obviates sample preparation because ratios
of analyte/internal standard remain constant in the presence
of extensive matrix effects. This MS method provided sufficient
sensitivity and selectivity for the rapid identification of fentanyl
and norfentanyl in urine at levels ≥ 10 ng/mL without prior
analyte resolution by chromatography and with a total analysis
time of less than 1 h.
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