Published:Journal of Chromatographic Science,
ISSN 0021-9665Volume
40, Number 1, January 2002, pp. 40-44
A Rapid and Sensitive High-Performance Liquid Chromatography–Electrospray
Ionization–Triple Quadrupole Mass Spectrometry Method for the Quantitation
of Oxycodone in Human Plasma
Michael Dawson[1], Bronwyn
Fryirs[2], Tamsin Kelly1, Jim Keegan[1], and Laurence E. Mather[2]
[1]Department of Chemistry, Materials and Forensic Science, University of Technology,
Sydney, P.O. Box 123, Broadway, N.S.W. 2007, Australia and
[2]Department of Anaesthesia and Pain Management, University of Sydney, Royal
North Shore Hospital, St. Leonards, N.S.W. 2065, Australia
A sensitive method for the determination of oxycodone concentrations
in plasma by high-performance liquid chromatography (HPLC)–electrospray
ionization–triple quadrupole mass spectrometry is described. The method
is rugged, reliable, selective, and rapid with a run time of 2 min. One milliliter
of plasma is made basic and extracted with 2-mL duplicate portions of 2% isoamyl
alcohol in n-butyl chloride. The combined extracts are then evaporated to dryness,
reconstituted in 100 µL of the mobile phase (15% methanol–85% water
containing 0.1% acetic acid), and injected onto the HPLC. The limit of quantitation
is 1 ng/mL, and the estimated limit of detection is 33 pg/mL (signal-to-noise
= 3). Standard curves are linear over the range of 1 to 100 ng/mL with all correlation
coefficient values greater than 0.9989. The method is used to determine the
concentration of oxycodone in human plasma following the intravenous infusion
of doses ranging from 5 to 15 mg in which the analysis of over 3000 plasma samples
is required.
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