用UHPLC-MS/MS法测定比格犬血浆中拉西地平的浓度  

Determination of lacidipine in Beagle dog plasma by UHPLC-MS/MS method

作　　者：王燕燕 姜宜宏 赵小英 周真宇 李晓红[2] 阎成炟 秦峰[1] WANG Yan-yan;JIANG Yi-hong;ZHAO Xiao-ying;ZHOU Zhen-yu;LI Xiao-hong;YAN Cheng-da;QIN Feng(School of Pharmaceutical,Shenyang Pharmaceutical University,Benxi 117000,Liaoning Province,China;Department of Pharmacy,The First Affiliated to China Medical University,Shenyang 110001,Liaoning Province,China;Drug Clinical Trial PhaseⅠCenter,The First Affiliated to China Medical University,Shenyang 110001,Liaoning Province,China)

机构地区：[1]沈阳药科大学药学院,辽宁本溪117000 [2]中国医科大学附属第一医院药学部,辽宁沈阳110001 [3]中国医科大学附属第一医院药物临床试验Ⅰ期中心,辽宁沈阳110001

出　　处：《中国临床药理学杂志》2024年第20期3038-3041,共4页The Chinese Journal of Clinical Pharmacology

基　　金：沈阳药科大学中青年教师事业发展支持计划基金资助项目(ZQN202305)。

摘　　要：目的建立一种测定比格犬血浆中拉西地平的超高效液相色谱-串联质谱方法。方法用蛋白沉淀法进行预处理,内标为尼莫地平。色谱柱:ACQUITY UPLC^(®)BEH C_(8)(2.1 mm×50.0 mm,1.7μm),流动相:100%水含5 mmol·L^(-1)醋酸铵-100%乙腈,流速:0.7 mL·min^(-1),柱温:40℃,自动进样器温度:4℃,进样量:20μL。用电喷雾离子化源,正离子模式,多反应监测。考察该方法的专属性、残留效应、标准曲线与定量下限、精密度与回收率、基质效应、稳定性。结果拉西地平在0.10~50.0 ng·mL^(-1)内线性关系良好,r=0.9966,定量下限为0.10 ng·mL^(-1),专属性良好,批内和批间相对标准偏差不超过12%,提取回收率高于80%,稳定性结果良好。结论本方法灵敏度高、操作简单、分析时间短,适用于比格犬血浆中拉西地平的药代动力学研究。Objective To establish an ultra high performance liquid chromatography-tandem mass spectrometry method for the determination of lacidipine in plasma of beagle dogs was established.Methods It was pretreated by protein precipitation method and the internal standard was nimodipine.Chromatographic column:ACQUITYUPLC^(®)BEH C_(8)(2.1 mm×50.0 mm,1.7μm),mobile phase:100%water containing 5 mmol·L^(-1)ammonium acetate-100%acetonitrile,flow rate:0.7 mL·min^(-1),column temperature:40℃,automatic injector temperature:4℃,injection volume:20μL.Electrospray ionization source,positive ion mode,multi-reaction monitoring.The specificity,residual effect,standard curve and quantitative lower limit,precision and recovery,matrix effect and stability of the method were investigated.Results Lacidipine has a good linear relationship in the range of 0.10-50.0 ng·mL^(-1),r=0.9966,the lower limit of quantification was 0.10 ng·mL^(-1).The specificity was good.The intra-and inter-relative standard deviation was less than 12%.The extraction recovery was higher than 80%,and the stability was good.Conclusion The method has the advantages of high sensitivity,simple operation and short analysis time,and was suitable for the pharmacokinetic study of lacidipine in Beagle dog plasma.

关 键 词：拉西地平 超高效液相色谱-串联质谱法 血药浓度 

分 类 号：R972[医药卫生—药品]