Zhao Ying, Zhai Desheng, Chen Xijing, Yu Qiaoling, He Hui, Sun Ya, Gao Zidong, Wang Lei, Wang Huanhuan, Han De'en, Ji Hui
School of Pharmacy, China Pharmaceutical University, Nanjing, 210009, China.
J Chromatogr Sci. 2010 Feb;48(2):81-5. doi: 10.1093/chromsci/48.2.81.
A simple, specific, and precise liquid chromatographic-electrospray ionization mass spectrometric (LC-ESI-MS) method has been developed for determination of nimodipine concentration in human plasma. The method involves the addition of 200 microL of saturated sodium bicarbonate (NaHCO(3)) solution to plasma to improve the extraction recovery, liquid-liquid extraction of nimodipine from plasma samples with anhydrous diethyl ether, simple reversed-phase chromatography, and ESI mass spectrometric detection in negative ion selected ion monitoring mode (SIM) using target [M-] ions at m/z 417 and m/z 359 for nimodipine and nitrendipine (internal standard, IS), respectively. A complete analytical run was achieved within 3.5 min. The limit of quantification was 0.5 ng/mL. The method was validated within a linear range of 0.5-100 ng/mL. The correlation coefficient for the calibration regression line was 0.9995 or better. Intra- and inter-batch accuracy and precision were acceptable. Analyte was stable in a battery of stability studies. The method has been successfully used in a bioequivalence study.
已开发出一种简单、特异且精确的液相色谱 - 电喷雾电离质谱（LC - ESI - MS）方法，用于测定人血浆中尼莫地平的浓度。该方法包括向血浆中加入200微升饱和碳酸氢钠（NaHCO₃）溶液以提高提取回收率，用无水乙醚对血浆样品中的尼莫地平进行液 - 液萃取，简单的反相色谱法，以及在负离子选择离子监测模式（SIM）下进行ESI质谱检测，分别使用m/z 417处的目标[M - ]离子测定尼莫地平，使用m/z 359处的目标[M - ]离子测定尼群地平（内标，IS）。在3.5分钟内完成一次完整的分析运行。定量限为0.5纳克/毫升。该方法在0.5 - 100纳克/毫升的线性范围内得到验证。校准回归线的相关系数为0.9995或更高。批内和批间的准确度和精密度均可接受。在一系列稳定性研究中，分析物是稳定的。该方法已成功用于生物等效性研究。
