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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 26, Number 7, October 2002,
pp. 524-528
Simultaneous Quantitation of Opioids in Blood by GC–EI-MS
Analysis Following Deproteination, Detautomerization of Keto Analytes, Solid-Phase
Extraction, and Trimethylsilyl Derivatization
Jeri D. Ropero-Miller[1], Matthew K. Lambing[2],
and Ruth E. Winecker[1]
[1]Office of the Chief Medical Examiner, Chapel Hill, North Carolina
[2]Southwestern Institute of Forensic Sciences, Dallas, Texas
Seven opioid analytes including
codeine, morphine, 6-acetylmorphine, hydrocodone, hydromorphone, oxycodone,
and oxymorphone were detected in postmortem blood (n > 1000). Two milliliters
of specimen was deproteinated with ~ 2.5 mL of methanol and derivatized with
hydroxylamine before solid-phase extraction and derivatization with BSTFA +
1% TMCS. Extracts were assayed by gas chromatography–electron impact-mass
spectrometry utilizing selected ion mode. One-microliter aliquots were injected
onto an HP-1MS capillary column (30 m x 0.25-mm i.d., 0.25 µm) with a
helium linear velocity of 62 cm/s. Temperature programming began at 160°C
(hold 0 min), then increased at rates of 35°C/min to 195°C, 5°C/min
to 240°C, and 30°C/min to 300°C (hold 2 min) resulting in a total
run time of 14-min. Quantitative determinations were based on the ratios of
the analyte peak areas to the corresponding deuterated analogues. Calibration
curves were linear for the following concentrations: 10–500 ng/mL (6-AM),
100–2000 ng/mL (oxycodone), and 50–1000 ng/mL (all other opioids).
LOQs ranged from 5 ng/mL (6-AM) to 20 ng/mL (oxycodone). Between-run precision
yielded CVs ranging from 2.79% to 5.34% (n = 12). These data suggest that methanolic
deproteination and dual derivatization improve separation and simultaneous quantitation
of seven opioid analytes in difficult matrices. Reproduction
of editorial content of this journal is prohibited without publisher’s
permission.
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