SENSITIVE CAPILLARY GAS-CHROMATOGRAPHIC MASS-SPECTROMETRIC SELECTED-ION MONITORING METHOD FOR THE DETERMINATION OF DICLOFENAC CONCENTRATIONS IN HUMAN PLASMA
Mr. Borenstein et al., SENSITIVE CAPILLARY GAS-CHROMATOGRAPHIC MASS-SPECTROMETRIC SELECTED-ION MONITORING METHOD FOR THE DETERMINATION OF DICLOFENAC CONCENTRATIONS IN HUMAN PLASMA, Journal of chromatography B. Biomedical applications, 685(1), 1996, pp. 59-66
Citations number
19
Categorie Soggetti
Chemistry Analytical","Biochemical Research Methods
Journal title
Journal of chromatography B. Biomedical applications
We have modified and validated a capillary GC-MS method reported by Ka
dowaki et al. [J. Chromatogr, 308 (1984) 329] for the determination of
diclofenac in human plasma by using heptane rather than benzene as an
extraction agent. In addition, acetone was added to the samples as a
deproteination agent which increased the recovery of diclofenac. These
revised processes allowed clean extraction and near-quantitative reco
very of analyte (>95%). Separation was achieved on an HP-I column with
helium as carrier gas. The parent ion peaks of diclofenac (m/z 277) a
nd the internal standard, 4'-methoxydiclofenac (m/z 307), were monitor
ed by a mass-selective detector using the selected-ion monitoring mode
. The linear range for the routine assay was from 5 to 2000 ng/ml. The
detection and lower quantifiable limits were 0.2 and 1 ng/ml, respect
ively, with no interference from plasma. The within-day and between-da
y coefficients of variation for high and medium concentrations were le
ss than 5% and were less than 13% for low concentrations (IO ng/ml). T
his GC-MS assay method has been used for pharmacokinetic and drug inte
raction studies in humans.