高效液相色谱方法同时测定土壤中4种水溶性抗凝血杀鼠药

Simultaneous Determination of Four Water-soluble Anticoagulant Rodenticides in Soil by High Performance Liquid Chromatography

[目的]建立同时测定土壤中溴敌隆、杀鼠醚、杀鼠灵和敌鼠钠盐4种主要水溶性抗凝血杀鼠药的高效液相色谱检测方法。[方法]土壤中的4种鼠药经过乙腈与水混合溶剂超声波辅助萃取,过滤后用乙腈和0.01mol/L乙酸铵缓冲溶液进行梯度洗脱,ZorbaxEclipsePlusC18柱分离,于波长306和265nm处用紫外检测器检测,外标法定量。[结果]溴敌隆、杀鼠醚、杀鼠灵和敌鼠钠盐在0.1~10.0μg/mL线性关系良好,方法检出限为0.1mg/kg,方法的加标回收率为91.3%~103.1%,各物质相对标准偏差<2.5%。[结论]该方法的回收率与方法精密度良好,适用于土壤中溴敌隆、杀鼠醚、杀鼠灵和敌鼠钠盐的测定。

[Objective]The research aimed to establish a high performance liquid chromatography method for the simultaneous determination of four major water-soluble anticoagulant rodenticides in the soil, such as bromadiolone, coumatetralyl, warfarin and diphacinone-Na.[Method]The four murine drugs in the soil were ultrasonically assisted extraction by acetonitrile and water mixed solvent.After filtration, the gradient was eluted with acetonitrile and 0.01 mol/L ammonium acetate buffer solution, separated by Zorbax Eclipse Plus C 18 column, detected by ultraviolet detector at wavelengths of 306 and 265 nm, and quantified by external standard method.[Result]The calibration curve was linear in the range of 0.1-10.0 μg/mL, and the detection limit of the method was 0.10 mg/kg. The matrix recoveries was from 91.3% to 103.1%, and the relative standard deviations were less than 2.5%.[Conclusion]The method has good recovery rate and method precision, and is suitable for the determination of bromadiolone, coumatetralyl, warfarin and diphacinone-Na in soil.