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机构地区:[1]j苏州大学附属第一医院,江苏苏州215006
出 处:《中国药房》2012年第46期4355-4358,共4页China Pharmacy
摘 要:目的:建立测定人血浆中硝苯地平浓度的方法。方法:采用液-液萃取法处理血浆后以超高效液相色谱-串联质谱法进样测定。色谱柱为WatersAcquityUPLCBEHC18,流动相为甲醇-10mmol·mL-1甲酸铵水溶液(85∶15),流速为0.2mL·min-1,正离子多离子反应监测(MRM)扫描分析,离子通道分别为m/z347.14→315.15(硝苯地平)、m/z384.10→338.10(非洛地平)。结果:硝苯地平血药浓度在1~200ng·mL-1范围内线性关系良好(r=0.9980),定量下限为1ng·mL-1,提取回收率为68.2%~71.2%,方法回收率为94.0%~106.5%,日内、日间RSD均<11%。结论:本方法操作简便、快速、特异性强、灵敏度高,可用于硝苯地平的药动学研究。OBJECTIVE: To establish a method for the determination of nifedipine concentration in human plasma. METHODS: The plasma procedure involved a single-step liquid-liquid extraction, then chromatographed on a Waters Acquity UPLC BEH C18 column with mobile phase consisted of methanol-10 mmol·mL-1 ammonium formate (85∶15) at the flow rate of 0.2 mL·min-1. The protonated ions of analytes were detected in positive ionization in multiple reaction monitoring mode (MRM). The mass transition pairs of m/z 347.14→315.15 and m/z 384.10→338.10 were used to detect nifedipine and felodipine. RESULTS: The linear range of nifedipine was 1~200 ng·mL-1 (r=0.998 0) and the lowest limit of quantitation was 1 ng·mL-1. The extraction recovery rates were ranged from 68.2% to 71.2%, and method recoveries were 94.0%~106.5%. RSDs of intra-day and inter-day were all less than 11%. CONCLUSION: The method is simple, quick, specific and sensitive, and suitable for the pharmacokinetics research of nifedipine.
关 键 词:硝苯地平 超高效液相色谱-串联质谱法 药动学 血药浓度
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