Full-scan high resolution accurate mass spectrometry (HRMS) in regulated bioanalysis: LC–HRMS for the quantitation of prednisone and prednisolone in human plasma

作者: Eliza N. Fung , Yuan-qing Xia , Anne-Francoise Aubry , Jianing Zeng , Timothy Olah

DOI: 10.1016/J.JCHROMB.2011.08.025

关键词: ChemistryChromatographyAnalytical chemistryMass spectrometryBioanalysisPlasma samplesHuman plasmaExtraction (chemistry)PrednisoloneHigh resolutionAnalyte

摘要: Abstract A liquid chromatography–full scan high resolution accurate mass spectrometry (LC–HRMS) method for quantifying prednisone and prednisolone in human plasma using a quadrupole time-of-flight spectrometer (Q-TOF) was developed. Plasma samples were extracted liquid–liquid extraction procedure. Full data acquired the TOF only mode ion chromatograms generated post-acquisition with exact masses of analytes. The calibration range 5–2500 ng/mL, Lower Limit Quantitation (LLOQ) 5 ng/mL. assay accuracy between 98.4% 106.3%. between-run (inter-day) within-run (intra-day) precision within 1.7% 2.9%, respectively. matrix effect 0.98 1.10 six different lots evaluated. Pooled incurred analyzed by results matched those obtained from an LC–MS/MS method. In addition, qualitative information on phospholipids, other endogenous components also full-scan acquired.

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