Qi Meiling, Wang Peng, Jin Xin
Department of Chemistry, School of Science, Beijing Institute of Technology, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Jan 2;830(1):81-5. doi: 10.1016/j.jchromb.2005.10.035. Epub 2005 Nov 8.
A simple and sensitive liquid chromatography-mass spectrometry method is described for the determination of nicardipine in human plasma. Chromatographic separation of the analyte was achieved on a C(18) column using a mobile phase of methanol, water and formic acid (320:180:0.4, v/v/v). Selected ion monitoring (SIM) in positive mode was used for analyte quantification at m/z 480.2 for nicardipine and m/z 256.4 for diphenhydramine. The run time was less than 5 min. The linearity over the concentration range of 0.05-20.0 ng/ml for nicardipine was obtained and the lower limit of quantification was 0.05 ng/ml. For each level of QC samples, inter-day and intra-day precisions (R.S.D.) were < or =9.3 and 11.1%, respectively, and accuracy (RE) was +/-4.9%. The present LC-MS method was successfully applied in the pharmacokinetic studies of nicardipine hydrochloride delayed-release tablets in two formulations after oral administration to healthy volunteers.
描述了一种简单且灵敏的液相色谱-质谱法用于测定人血浆中的尼卡地平。在C(18)柱上，以甲醇、水和甲酸（320:180:0.4，v/v/v）的流动相实现了分析物的色谱分离。采用正离子模式下的选择离子监测（SIM）对分析物进行定量，尼卡地平的质荷比为480.2，苯海拉明的质荷比为256.4。运行时间少于5分钟。获得了尼卡地平在0.05 - 20.0 ng/ml浓度范围内的线性关系，定量下限为0.05 ng/ml。对于每个质量控制样品水平，日间和日内精密度（相对标准偏差）分别≤9.3%和11.1%，准确度（相对误差）为±4.9%。本液相色谱-质谱法成功应用于健康志愿者口服两种制剂的盐酸尼卡地平缓释片的药代动力学研究。
