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Title

Low picogram determination of Ro 48-6791 and its major metabolite, Ro 48-6792, in plasma with column-switching microbore high-performance liquid chromatography coupled to ion spray tandem mass spectrometry

Authors
Zell, M.
Husser, C.
Published in Rapid Communications in Mass Spectrometry. 1997, vol. 11, no. 10, p. 1107-14
Abstract A coupled liquid chromatography/tandem mass spectrometry assay was developed for simultaneous determination of Ro 48-6791 and its secondary amine metabolite in human plasma samples with a quantification limit for both compounds of 1 pg/mL using a 1 mL plasma aliquot. The method exploits the enhanced mass sensitivity of a microbore (300 microns i.d.) reversed-phase capillary column coupled to an ion spray probe combined with tandem mass spectrometry. A straightforward column-switching system was utilized to focus the analytes onto a microbore trapping column following solid-phase extraction of a 50 microL plasma sample extract from liquid/liquid extraction. Backflushing of the retained analytes from the trapping column onto the microbore capillary column provided the requisite high peak concentration for high sensitivity. The inter-assay precision and accuracy for Ro 48-6791 and its metabolite, at 10 pg/mL, were found to be 3.4%, and 105%, and 9.1%, and 99.9%, respectively. The calibration curves were linear over the range 1 to 1000 pg/mL. The method proved to be sufficiently rugged for analysis of samples.
Keywords Anti-Anxiety AgentsBenzodiazepines/bloodCalibrationChromatography, High Pressure Liquid/methodsHumansMass Spectrometry/methodsMolecular StructureReproducibility of Results
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PMID: 9218357
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ZELL, M., HUSSER, C., HOPFGARTNER, Gerard. Low picogram determination of Ro 48-6791 and its major metabolite, Ro 48-6792, in plasma with column-switching microbore high-performance liquid chromatography coupled to ion spray tandem mass spectrometry. In: Rapid Communications in Mass Spectrometry, 1997, vol. 11, n° 10, p. 1107-14. https://archive-ouverte.unige.ch/unige:2313

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Deposited on : 2009-08-04

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