【摘要】 目的建立全血中测定溴敌隆的高效液相色谱-电喷雾-质谱联用检测方法。方法血液样品经乙醚提取后,采用UltraC18柱(150 mm×2.1mm×5μm);柱温:23℃;流动相:甲醇;流速:200μl/min;在负离子模式下,通过电喷雾电离(ESI),多反应监测(MRM)测定,外标法定量分析溴敌隆。结果在0.1～50mg/l范围内两者均呈良好的线性关系。溴敌隆的回收率为94.34%(RSD=7.3%),考察了方法的基质抑制作用(matrix effect,ME)(%)=B/A×100%=91.86%(RSD=4.78%)定量检出限为0.028ng。结论本方法简便、灵敏度高、定性定量准确,可以作为检验全血中溴敌隆检验的一种手段。更多还原

【Abstract】 Objective To establish a HPLC-ESI-MS/MS method for determination of Bromadiolone in whole blood.Methods After Bromadiolone in whole blood were extracted by ethyl acetate,the samples were separated on Restek Ultra C18(150 mm×2.1 mm×5μm) at a constant temperature of 23℃ by using CH3OH as a mobile phase.The flow rate was 200μl/min.Detection was performanced on an electrospray ionization(ESI) in the negative mode.Results Calibration curves were linear within the range of 0.1～50mg/land the limit of quantitation was found to be 0.028ng.The extraction recovery were 94.34% and the RSD were 7.3%.Conclusion This method is simple,sensitive and accurate for the determination of Bromadiolone in poisoncases.更多还原