Liquid–liquid extraction was followed by high-performance liquid Full scan ESI mass spectrum of oxycodone, noroxycodone and.
All tubes were vortexed briefly, and 4 mL of 4:1 n -butyl chloride:acetonitrile was added. The organic solvent was evaporated off under 10 psi air at 40°C in a Zymark Turbo Vap evaporator. The residues were reconstituted in 75 µL of 0.1% formic acid in Milli-Q water and transferred into autosampler vials. Urine (200 µL) was incubated with 200 µL of 0.1 M sodium acetate buffer (with 5000 units/mL β-glucuronidase, pH 5) at 50°C for 16 h. Aliquots of 1.0 mL (for plasma and HLM) or 200 µL (for urine) of quality control (QC) samples, calibration standards and study samples were added to silanized tubes.
FULL TEXT Abstract: The opioid analgesic oxycodone is widely abused Liquid–liquid extraction was followed by high-performance liquid.
In urine (both nonhydrolyzed and hydrolyzed), it ranged from 0.25 to 7.21% with a mean of 2.41% for oxycodone, from 1.73 to 12% with a mean of 4.75% for oxymorphone and from 0.93 to 6.80% with a mean of 2.43% for noroxycodone. In samples with no additions, peak heights at the retention time of the d 0 -analytes were not visible and similar to those with only internal standards added, excluding the contribution to the d 0 -analyte peak from the internal standard. Mean ratios relative to the mean LLOQ ranged from 1.04 to 4.51% with a mean of 1.92% for oxycodone, from 1.98 to 8.18% with a mean of 4.28% for oxymorphone and from 8.63 to 16.6% with a mean of 11.4% for noroxycodone in human plasma.
A sensitive analytical method was developed for oxycodone and its metabolites, Liquid-liquid extraction was followed by high-performance liquid.
T1 - Determination of oxycodone, noroxycodone and oxymorphone by high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry in human matrices.
T2 - Journal of Analytical Toxicology.
AU - Lofwall,Michelle R.
; Moody, David E. / Determination of oxycodone, noroxycodone and oxymorphone by high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry in human matrices : In vivo and in vitro applications. Fang, Wenfang B.; Lofwall, Michelle R.; Walsh, Sharon L.
Research output : Contribution to journal › Article } TY - JOUR.
Walsh ; David E.
Peak fronting in reversed-phase high-performance liquid chromatography: a study of the chromatographic behavior of oxycodone hydrochloride. Broglé K(1).
National Library of Medicine 8600 Rockville Pike, Bethesda MD, 20894 USA. National Center for Biotechnology Information, U.S.
Severe peak asymmetry--fronting--was observed for oxycodone during elution at 30 degrees C from a C18 HPLC column using a mobile phase consisting of 14.9% MeOH, 84.5% 0.05 M KH2PO4 (pH 3.0), 0.5% MTBE, and 0.1% TEA. Increasing the column temperature to 60 degrees C increased the rates of interconversion with the result that the three species eluted as a single, homogenous peak with greatly improved peak symmetry. Decreasing the column temperature to 0 degrees C decreased the rates of interconversion and allowed the resolution and separation of these species from each other and from oxycodone. Investigation using deuterium-labeled oxycodone and analysis by LC/MS showed that gem diol and hemiketal adducts of oxycodone formed as a result of the equilibrium addition of water and methanol to the C-6 ketone on oxycodone. As a result of slow equilibrium kinetics at room temperature in aqueous solution, the gem-diol and methyl hemiketal eluted as an unresolved broad band in front of the oxycodone peak.
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2099 Note Determination of oxycodone in human plasma by high.performance liquid chromatography with electrochemical detection JENNY J. SCHNEIDER.
Received 16 November 1983, Revised 27 January 1984, Available online 27 December 2002.
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Journal of Chromatography B: Biomedical Sciences and Applications.
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Volume 308, 8 June 1984, Pages 359-362 Note.
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1984 Published by Elsevier B.V. OpenAthens login Other institution login.