【摘要】 目的:建立大鼠体内去甲基斑蝥素的 HPLC-MS 分析方法。方法:选用烟尿酸为内标,血浆样品经乙腈沉淀蛋白处理。色谱条件为 Hypersil SAX 阴离子交换色谱柱（4.6mm×250mm,5μm）,甲醇-水（25∶75,含2.5%甲酸）为流动相,流速0.5mL·min^-1,采用 HPLC-MS检测系统,AP-ESI 负离子模式,质谱检测参数如下:AP-ESI 负离子模式;雾化压力276kPa;温度350℃;保护气流量8 L·min^-1;毛细管电压3500V;裂解电压为90V（NCTD）和120V（内标）;SIM 检测,NCTD m/z185（M+H₂O-H）、烟尿酸m/z 179（M-H）。结果:血浆中去甲基斑蝥素检测方法的线性范围为0.2-20μg·mL^-1,最低检测限可达2ng·mL^-1。血浆中去甲基斑蝥素的平均回收率为96.7%-100.3%,日内、日间 RSD 均小于8%。结论:本法灵敏、准确、选择性高,可用于去甲基斑蝥素的药代动力学研究。更多还原

【Abstract】 Objective:To establish an HPLC-MS method for the determination of norcantharidin in rat plasma. Method:The plasma was precipitated with acetonitrile and the internal standard was nicotinoylglycine.A SAX col- umn was used to separate norcantharidin in plasma with a mixture of methanol-water（25:75,containing 2.5% for- mic acid）as mobile phase at flow rate of 0.5mL min^-1.The analysis was detected by the negative electrospray ioni- zation（ESI^-）-MS method under selected-ion monitoring（SIM）mode.The MS detection parameters was set as follows:the nebulizer pressure was 276 kPa,the temperature was 350℃,the drying gas flow was 8L·min^-1,the capillary voltage was 3500V,the fragmentor was 90V（norcantharidin）and 120V（internal standard）,the SIM ions were m/z 185（norcantharidin,M+H₂O-H）and m/z 179（internal standard,M-H）.Results:The linear range of the standard curve of norcantharidin was 0.2-20μg·mL^-1,and the test limit was 2ng·mL^-1.The recovery was 96.7%-100.3%,intra-day and inter-day RSD were less than 8%.Conclusion:The method had high sensitiv- ity,good selectivity and precision.It is suitable for determination of the norcantharidin in plasma.更多还原