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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 establish a rapid and sensitive liquid chromatography-tandem mass spectrometry method for the determination of nisoldipine in human plasma. Methods: The plasma samples were extracted by liquid-liquid n-hexane-dichloromethane-isopropanol (20:10:1) using acetonitrile-water-formic acid (90:10:0.1) as mobile phase and Zorbax C8 × 4.6 mm, 5 μm) column. Atmospheric pressure chemical ionization sources are used for detection in multiple reaction monitoring (MRM) mode. The ion reactions used for the quantitative analysis were m / z 389.2 → 315.2 (nisoldipine) and m / z 419.2 → 343.2 (internal standard nimodipine), respectively. RESULTS: The linear range of nisoldipine in plasma was 0.020-8.00 ng · mL-1 with a lower limit of quantification of 0.020 ng · mL-1. The RSDs were both less than 7.6% and the accuracy (RE) Between -3.4% and 5.7%, the single sample analysis time was 3.0 min. This method has been used to study the bioequivalence of oral nisoldipine test and reference preparations in healthy subjects. Conclusion: The method has high sensitivity, strong selectivity and short analysis time. It is suitable for the determination of nisoldipine in human plasma samples.