Zhang Zunjian, Tian Yuan, Ni Li, Li Jinheng
Center for Instrumental Analysis, China Pharmaceutical University, Nanjing 210009, PR China.
J Chromatogr Sci. 2004 Oct;42(9):501-5. doi: 10.1093/chromsci/42.9.501.
A selective and sensitive high-performance liquid chromatography-electrospray ionization mass spectrometry (MS) for the determination of nisoldipine in human plasma is first presented. With nimodipine as the internal standard, nisoldipine is extracted from plasma with ethyl acetate. The organic layer is evaporated and the residue is resuspended in the mobile phase of methanol-water (80:20, v/v). An aliquot of 40 microL is chromatographically analyzed on an Agilent ODS C18 reversed-phase column (5 microm, 250- x 4.6-mm i.d.) by means of selected-ion monitoring mode MS. The calibration curve of nisoldipine in plasma exhibits a linear range from 0.5 to 20.0 ng/mL with a correlation coefficient of 0.9995. The limit of detection is 0.2 ng/mL. The within- and between-day variations (relative standard deviation) are less than 9.28% and 11.13% (n = 5), respectively. The developed method is validated through successful use for the analysis of nisoldipine contained in biological fluids resulting from a phase-I human pharmacokinetic study.
首次提出了一种用于测定人血浆中尼索地平的选择性和灵敏的高效液相色谱 - 电喷雾电离质谱法（MS）。以尼莫地平为内标，用乙酸乙酯从血浆中萃取尼索地平。将有机层蒸发，残渣重新悬浮于甲醇 - 水（80:20，v/v）流动相中。取40 μL 等分试样，在安捷伦ODS C18反相柱（5 μm，250×4.6 mm内径）上通过选择离子监测模式MS进行色谱分析。血浆中尼索地平的校准曲线线性范围为0.5至20.0 ng/mL，相关系数为0.9995。检测限为0.2 ng/mL。日内和日间变化（相对标准偏差）分别小于9.28%和11.13%（n = 5）。所建立的方法通过成功用于分析一期人体药代动力学研究所得生物流体中所含的尼索地平而得到验证。
