Chromatography Research Today is a free monthly online journal that collates and summarizes the latest research about Chromatography, including details on column chromatography, gas chromatography (gc), liquid chromatograpy, hplc. | ||||||||
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Determination of cilnidipine, a new calcium antagonist, in human plasma using high performance liquid chromatography with tandem mass spectrometric detection.Zhang X, Zhai S, Zhao R, Ouyang J, Li X, Baeyens WR Peking University Third Hospital, Peking University TDMCT Center, Beijing 100083, PR China. A rapid, sensitive and reliable high performance liquid chromatographic method coupled with tandem mass spectrometry (HPLC-MS/MS) has been developed and validated for the determination of cilnidipine, a relatively new calcium antagonist, in human plasma. The reversed-phase chromatographic system was interfaced with a TurboIonSpray (TIS) source. Nimodipine was employed as the internal standard (IS). Sample extracts following protein precipitation were injected into the HPLC-MS/MS system. The analyte and IS were eluted isocratically on a C18 column, with a mobile phase consisting of CH(3)OH and NH(4)Ac (96:4, v/v). The ions were detected by a triple quadrupole mass spectrometric detector in the negative mode. Quantification was performed using multiple reaction monitoring (MRM) of the transitions m/z 491.2-->122.1 and m/z 417.1-->122.1 for cilnidipine and for the IS, respectively. The analysis time for each run was 3.0 min. The calibration curve fitted well over the concentration range of 0.1-10 ngmL(-1), with the regression equation Y=(0.103+/-0.002)X+(0.014+/-0.003) (n=5), r=0.9994. The intra-day and inter-day R.S.D.% were less than 12.51% at all concentration levels within the calibration range. The recoveries were between 92.71% and 97.64%. The long-term stability and freeze-thaw stability were satisfying at each level. The present method provides a modern, rapid and robust tool for pharmacokinetic studies of cilnidipine. Published 1 October 2007 in Anal Chim Acta, 600(1): 142-6.
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