HPLC-ESI-MS/MS法分析肝组织中4种杀鼠剂

目的建立测定杀鼠迷、杀鼠灵、溴敌隆和大隆4种杀鼠剂的高效液相色谱电喷雾质谱联用检测方法。方法采用ZORBAX sb-aq,150mm×2.1mm×3.5μm(带预柱);柱温:30℃;流动相:甲酸(0.1%)甲醇和甲酸(0.1%)水溶液梯度条件;流速:0.4 mL/min;在负离子模式下,通过电喷雾电离(ESI),多反应离子监测(MRM)测定,外标法定量分析4种杀鼠剂,并测试方法的基质抑制作用。结果4种鼠药在MRM筛选条件下,最小检出均在40pg以下;单个鼠药线性相关系数均在0.999以上,线性范围适当,最小检出限均在10pg以下。结论本实验方法可以作为检验生物检材中杀鼠迷、杀鼠灵、溴敌隆和大隆的筛选手段。

The determination of four kinds of rodenticides in liver tissue by HPLC-ESI-MS/MS

Objective To set up a determination method of warfarin,coumatertralyl,bromadiolone and brodifacoum.Methods HPLC-ESI-MS/MS was used to detect warfarin,coumatertralyl,bromadiolone and brodifacoum using ZORBAX sb-aq(1 50mm×2.1 mm×3.5 μm)as chromatographic column at constant temperature 30℃ while methanol of 0.1%formic acid and water as mobile phase in the grads program.The flow rate was 0.4 mL/min;Detection was performed on an electrospray ionization(ESI)in the negative model and the MRM condition.Results The limit of qualitation was found to be less than 40 pg for four raticides at one time and 10pg for every raticide in the MRM condition;The four raticides linear range were suitable and r were more than 0.999.Matrix affection Was also determined.Conclusion This method is simple,sensitive and accurate for the determination of warfarin,coumatertralyl,bromadiolonc and brodifacoum in the biological tissue.