Determination of lercanidipine in human plasma by an improved UPLC–MS/MS method for a bioequivalence study  

作　　者：Darshan V.Chaudhary Daxesh P.Patel Priyanka A.Shah Jaivik V.Shah Mallika Sanyal Pranav S.Shrivastav 

机构地区：[1]Department of Chemistry, School of Sciences, Gujarat University, Navrangpura, Ahmedabad, Gujarat 380009, India [2]Laboratory of Metabolism, Center for Cancer Research, National Cancer Institute, National Institutes of Health, Building 37, Room 3106, Bethesda, MD 20892, USA [3]Department of Chemistry, St. Xavier's College, Navrangpura, Ahmedabad, Gujarat 380009, India

出　　处：《Journal of Pharmaceutical Analysis》2016年第2期87-94,共8页药物分析学报（英文版）

基　　金：UGC-BSR (F 4-1/2009 (BSR)/7-74/2007);New Delhi, for research fellowship, F 4-1/2009 (BSR)/7-74/2007;Department of Chemistry, Gujarat University, for supporting this work

摘　　要：An improved and reliable ultra-performance liquid chromatography/tandem mass spectrometry （UPLC- MS/MS） method has been developed and validated for the determination of lercanidipine in human plasma. Plasma samples with lercanidipine-d3 as an internal standard （IS） were prepared by solid phase extraction on Phenomenex Strata-X cartridges using 100 μL of human plasma. Chromatographic analysis was performed on UPLC BEH C18 （50 mm × 2.1 mm, 1.7 μm） column under isocratic conditions. Linear calibration curves were obtained over a wide dynamic concentration range of 0.010-20.0 ng/mL. Matrix effect was assessed by post-column infusion, post-extraction spiking and standard-line slope methods. The mean extraction recovery was 〉 94% for the analyte and IS. Inter-batch and intra-hatch precision （% CV） across five quality controls was 〈 5.8%. Bioequivalence study was performed with 36 healthy sub- jects after oral administration of 10 mg of lercanidipine and the assay reproducibility was evaluated by reanalysis of 133 incurred samples.An improved and reliable ultra-performance liquid chromatography/tandem mass spectrometry （UPLC- MS/MS） method has been developed and validated for the determination of lercanidipine in human plasma. Plasma samples with lercanidipine-d3 as an internal standard （IS） were prepared by solid phase extraction on Phenomenex Strata-X cartridges using 100 μL of human plasma. Chromatographic analysis was performed on UPLC BEH C18 （50 mm × 2.1 mm, 1.7 μm） column under isocratic conditions. Linear calibration curves were obtained over a wide dynamic concentration range of 0.010-20.0 ng/mL. Matrix effect was assessed by post-column infusion, post-extraction spiking and standard-line slope methods. The mean extraction recovery was 〉 94% for the analyte and IS. Inter-batch and intra-hatch precision （% CV） across five quality controls was 〈 5.8%. Bioequivalence study was performed with 36 healthy sub- jects after oral administration of 10 mg of lercanidipine and the assay reproducibility was evaluated by reanalysis of 133 incurred samples.

关 键 词：LERCANIDIPINE UPLC-MS/MS BIOEQUIVALENCE Solid phase extraction Human plasma 

分 类 号：R96[医药卫生—药理学]