A liquid chromatography-tandem mass spectrometric method (LC-MS/MS) for quantifying ilaprazole and its major metabolite in human plasma was developed and validated. Sample preparation was based on chloroform extractio...A liquid chromatography-tandem mass spectrometric method (LC-MS/MS) for quantifying ilaprazole and its major metabolite in human plasma was developed and validated. Sample preparation was based on chloroform extraction. Chromatography was performed on a C18 analytical column and the retention times were 1.2, 1.28 and 1.65 min for ilaprazole, ilaprazole sulfone and omeprazole (internal standard), respectively. The ionization was optimized using ESI (+) and enhanced selectivity achieved by tandem mass spectrometric analysis. The calibration curve ranged from 0.36 to 368.40 ng/mL and from 0.125 to 128.000 ng/mL for ilaprazole and ilaprazole sulfone, respectively. The intra-and inter-day precision (CV) were within 15%, and accuracy of ilaprazole and ilaprazole sulfone were within 80% to 120%. The analytes showed stable over the timescale of the whole procedure. The robustness of the method was demonstrated by good reproducibility of results obtained from the analysis of clinical samples.展开更多
文摘A liquid chromatography-tandem mass spectrometric method (LC-MS/MS) for quantifying ilaprazole and its major metabolite in human plasma was developed and validated. Sample preparation was based on chloroform extraction. Chromatography was performed on a C18 analytical column and the retention times were 1.2, 1.28 and 1.65 min for ilaprazole, ilaprazole sulfone and omeprazole (internal standard), respectively. The ionization was optimized using ESI (+) and enhanced selectivity achieved by tandem mass spectrometric analysis. The calibration curve ranged from 0.36 to 368.40 ng/mL and from 0.125 to 128.000 ng/mL for ilaprazole and ilaprazole sulfone, respectively. The intra-and inter-day precision (CV) were within 15%, and accuracy of ilaprazole and ilaprazole sulfone were within 80% to 120%. The analytes showed stable over the timescale of the whole procedure. The robustness of the method was demonstrated by good reproducibility of results obtained from the analysis of clinical samples.
