Validation of Blood and Liver Oxymorphone Analysis Using LC-MS-MS: Concentrations in 30 Fatal Overdoses
Author(s) -
E. D. Crum,
Keith Bailey,
Lauren L. RichardsWaugh,
D. J. Clay,
M. A. Gebhardt,
James C. Kraner
Publication year - 2013
Publication title -
journal of analytical toxicology
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.161
H-Index - 76
eISSN - 1945-2403
pISSN - 0146-4760
DOI - 10.1093/jat/bkt077
Subject(s) - chromatography , chemistry , detection limit , electrospray ionization , tandem mass spectrometry , analyte , mass spectrometry , ion suppression in liquid chromatography–mass spectrometry , calibration curve , oxymorphone , solid phase extraction , quantitative analysis (chemistry) , sample preparation , selected reaction monitoring , biochemistry , oxycodone , receptor , opioid
A sensitive liquid chromatography-tandem mass spectrometry method was developed and validated for the quantitation of oxymorphone (OM) in human whole blood and liver. Sample preparation was done by solid-phase extraction, using deuterated OM as the internal standard. Separation was achieved using a Waters Aquity UPLC HSS T3 column. Analysis utilized positive electrospray ionization and multiple reaction monitoring. As part of the validation, studies were conducted to determine potential interference, selectivity, ion suppression/enhancement and carryover. Calibration model, limit of detection (LOD), lower limit of quantitation (LLOQ), precision and accuracy were also established. The linear range of the method was 2-500 ng/mL in blood and 5-500 ng/g in the liver. The LOD and LLOQ were 2 ng/mL for blood and 5 ng/g for the liver. Blood and/or liver specimens from 30 cases were analyzed. OM concentrations ranged from 23 to 554 ng/mL ( , n = 26) in blood and 48 to 1740 ng/g ( , n = 30) in the liver.
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