Arapid,selective and sensitive liquid chromatography-tandem massspectrometry(LC-MS/MS)method has been developed and validated for the determination of pitavastatin in humanplasma.Following a liquid-liquid extraction,b...Arapid,selective and sensitive liquid chromatography-tandem massspectrometry(LC-MS/MS)method has been developed and validated for the determination of pitavastatin in humanplasma.Following a liquid-liquid extraction,both the analytes and internal standard telmisartan were separated on a Luna C_(18) column with a mobile phase consisted of acetonitrile-methanol-1% formic acid in water(50:25:25,v/v/v).Mass spectrometric detection involved electrospray ionization in the positive ion mode followed by multiple reaction monitoring(MRM)of the transitions at m/z 421.9→290.1 for pitavastatin and m/z 515.2→276.2 for the IS.The assay for pitavastatin showed good linearity(r≥0.99)over the ranges 0.2-400 ng/ml,with a lower limit of quantitation of 0.2 ng/ml.Accuracy and precision for the assay were determined by calculating the intra-and inter-batch variation of quality control(QC)samples at three concentration levels,with relative standard deviations(RSD)of less than 15%for both analytes.The mean extraction recovery of pitavastatin and IS were both above 70%.Matrix effect hasn't been found in this method.The method has been successfully applied to a clinic pharmacokinetic study of pitavastatin administered.展开更多
基金This work was supported by Qidu Pharmaceutical Co.,LTD(Zibo,China).
文摘Arapid,selective and sensitive liquid chromatography-tandem massspectrometry(LC-MS/MS)method has been developed and validated for the determination of pitavastatin in humanplasma.Following a liquid-liquid extraction,both the analytes and internal standard telmisartan were separated on a Luna C_(18) column with a mobile phase consisted of acetonitrile-methanol-1% formic acid in water(50:25:25,v/v/v).Mass spectrometric detection involved electrospray ionization in the positive ion mode followed by multiple reaction monitoring(MRM)of the transitions at m/z 421.9→290.1 for pitavastatin and m/z 515.2→276.2 for the IS.The assay for pitavastatin showed good linearity(r≥0.99)over the ranges 0.2-400 ng/ml,with a lower limit of quantitation of 0.2 ng/ml.Accuracy and precision for the assay were determined by calculating the intra-and inter-batch variation of quality control(QC)samples at three concentration levels,with relative standard deviations(RSD)of less than 15%for both analytes.The mean extraction recovery of pitavastatin and IS were both above 70%.Matrix effect hasn't been found in this method.The method has been successfully applied to a clinic pharmacokinetic study of pitavastatin administered.
