Journal of Separation Science · 2008 · 37 citations · 17 references
PharmacyPharmaceutical AnalysisPharmacologyAnalytical ChemistryChromatographic AnalysisMass Spectrometric AnalysisBioanalytical Method ValidationChromatographyClinical AnalysisInstrumental AnalysisLiquid ChromatographyMass SpectrometryConcentrationHydrophilic Interaction ChromatographyHydrophilic Interaction Chromatography ColumnsInternal Standard AnalysisLiquid Chromatography-mass SpectrometryLiquid Chromatography-mass Spectrometry AnalysisLiquid Chromatography-mass Spectrometry Method DevelopmentMass Spectrometric Drug Analysis
Hydrophilic interaction LC with MS/MS (HILIC-MS/MS) was described as a rapid, sensitive, and selective method for the quantification of doxazosin in human plasma. Doxazosin and cisapride (internal standard) were extracted from human plasma with ethyl acetate at alkaline pH and analyzed on an Atlantis HILIC Silica column with the mobile phase of ACN/ammonium formate (100 mM, pH 4.5) (93:7 v/v). The analytes were detected using an ESI MS/MS in the selective-reaction-monitoring mode. The standard curve was linear (r = 0.9994) over the concentration range of 0.2-50 ng/mL. The LOQ for doxazosin was 0.2 ng/mL using 100 microL plasma sample. The CV and relative error for intra- and interassay at four QC levels were 3.7-8.7% and 0.0-9.8%, respectively. The matrix effect for doxazosin and cisapride were practically absent. The recoveries of doxazosin and cisapride were 67.4 and 61.7%, respectively. This method was successfully applied to the pharmacokinetic study of doxazosin in humans.
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Angela Eerkes, Wilson Z. Shou, Naidong Weng · Journal of Pharmaceutical and Biomedical Analysis · 2003 · 57 citations