采用改进的超高效液相色谱-串联质谱法测定人血浆中乐卡地平用于生物等效性研究。
Determination of lercanidipine in human plasma by an improved UPLC-MS/MS method for a bioequivalence study.
作者信息
Chaudhary Darshan V, Patel Daxesh P, Shah Priyanka A, Shah Jaivik V, Sanyal Mallika, Shrivastav Pranav S
机构信息
Department of Chemistry, School of Sciences, Gujarat University, Navrangpura, Ahmedabad, Gujarat 380009, India.
Laboratory of Metabolism, Center for Cancer Research, National Cancer Institute, National Institutes of Health, Building 37, Room 3106, Bethesda, MD 20892, USA.
出版信息
J Pharm Anal. 2016 Apr;6(2):87-94. doi: 10.1016/j.jpha.2015.09.001. Epub 2015 Sep 28.
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 C (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-batch precision (% CV) across five quality controls was <5.8%. Bioequivalence study was performed with 36 healthy subjects after oral administration of 10 mg of lercanidipine and the assay reproducibility was evaluated by reanalysis of 133 incurred samples.
已开发并验证了一种改进的、可靠的超高效液相色谱/串联质谱法（UPLC-MS/MS），用于测定人血浆中的乐卡地平。以乐卡地平-d3作为内标（IS），使用100μL人血浆，通过在Phenomenex Strata-X柱上进行固相萃取来制备血浆样品。在UPLC BEH C（50mm×2.1mm，1.7μm）柱上于等度条件下进行色谱分析。在0.010 - 20.0 ng/mL的宽动态浓度范围内获得线性校准曲线。通过柱后注入、萃取后加样和标准曲线斜率法评估基质效应。分析物和内标的平均萃取回收率均>94%。五个质量控制样品的批间和批内精密度（%CV）均<5.8%。对36名健康受试者口服10mg乐卡地平后进行生物等效性研究，并通过对133个实际样品进行重新分析来评估分析方法的重现性。
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