液相色谱-串联质谱法测定人血浆中的尼索地平  

LC-MS/MS determination of nisoldipine in human plasma

作　　者：马金飞[1,2] 戴晓健[2] 陈笑艳[2] 钟大放[1,2] 

机构地区：[1]浙江工业大学,杭州310014 [2]中国科学院上海药物研究所,上海201203

出　　处：《药物分析杂志》2009年第10期1597-1601,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立快速、灵敏的液相色谱-串联质谱法测定人血浆中的尼索地平。方法:血浆样品经正己烷-二氯甲烷-异丙醇(20∶10∶1)液-液萃取后,以乙腈-水-甲酸(90∶10∶0.1)为流动相,采用Zorbax C8(150mm×4.6mm,5μm)柱分离。使用大气压化学电离源,以多反应监测(MRM)方式进行检测。用于定量分析的离子反应分别为m/z389.2→315.2(尼索地平)和m/z419.2→343.2(内标尼莫地平)。结果:测定血浆中尼索地平的线性范围为0.020～8.00ng·mL-1,定量下限为0.020ng·mL-1,日内、日间精密度(RSD)均小于7.6%,准确度(RE)在-3.4%～5.7%之间,单个样品分析时间为3.0min。本法已用于健康受试者口服尼索地平受试制剂和参比制剂后的生物等效性研究。结论:该法灵敏度高,选择性强,分析测试时间短,适用于人血浆样品中尼索地平的测定。Objective：To develop and validate a liquid chromatography -tandem mass spectrometric （LC -MS/ MS） method for the determination of nisoldipine in human plasma. Method：The plasma sample was extracted with n - hexane - dichlormethane - isopropanol （20： 10：1 ） ,then separated on a Zorbax Cs （ 150 mm×4.6mm,5μm）） column using acetonitrile -water -formic acid （90： 10： 0. 1 ） as the mobile phase. The triple quadrupole mass spec- trometry was applied via an atmospheric pressure chemical ionization （APCI） source for detection. Quantitation was performed using multiple reaction monitoring （MRM） of the transitions of m/z 389.2→315.2 and m/z 419.2→343.2 for nisoldipine and the internal standard nimodipine, respectively. Results：The linear calibration curves were obtained in the concentration range of 0. 020 - 8.00 ng·mL^-1. The lower limit of quantification was 0. 020 ng·mL^-1. The intra - day and inter - day relative standard deviation over the entire concentration range was less than 7.6%. The accuracy was in the range of - 3.4% to 5.7% in terms of relative error. Each sample was chromatographed within 3.0 min. The method is applied to evaluate the bioequivalence of two nisoldipine tablet formulations in healthy volunteers. Conclusion： This method is sensitive, selective, rapid and suitable for the determination of nisoldipine in human plasma.

关 键 词：尼索地平 液相色谱-串联质谱法 血浆药物浓度 

分 类 号：R917[医药卫生—药物分析学]