气相色谱-串联质谱法测定生物样品中3种杀鼠剂

目的　建立同时测定全血和尿中毒鼠强、氟乙酰胺和溴敌隆3种杀鼠剂的气相色谱-串联质谱测定法。方法　2022年5月至6月，在惠州市农产品质量安全监督检测中心实验室开展实验。于全血或尿液样品中加入适量氯化钠脱水，用乙酸乙酯萃取，采用GC-MS/MS法测定，利用特征离子定性，特征定量离子峰面积外标法定量。结果　该方法的检出限：毒鼠强为0.07 µg/ml（血）、0.10 µg/ml（尿）；氟乙酰胺为0.01 µg/ml（血）、0.02 µg/ml（尿）；溴敌隆为0.06 µg/ml（血）、0.04 µg/ml（尿）。方法的重现性好，相对标准偏差：毒鼠强为2.3%～8.1%，氟乙酰胺为2.2%～9.9%，溴敌隆为2.0%～6.4%。平均加标回收率：毒鼠强为81.5%～101.8%，氟乙酰胺为79.5%～103.2%，溴敌隆为87.6%～98.7%。结论　该方法检出限低，精密度和回收率好，适用于疑似鼠药中毒病人的全血和尿液样品中3种鼠药的测定。

Determination of three rodenticides in biological specimens by gas chromatography-tandem mass spectrometry

Objective　To establish a gas chromatography tandem mass spectrometry (GC-MS/MS) method for the simultaneous determination of rodenticides tetramine, fluoroacetamide, and bromadiolone in whole blood and urine. Methods　Form May to June 2022, the experiment was done in the laboratory of Huizhou Agricultural Product Quality and Safety Supervision and Testing Center. An appropriate amount of sodium chloride was added to the whole blood or urine samples for dehydration, extracted with ethyl acetate, determined by GC-MS/MS, qualitatively determined by characteristic ions, and quantitatively determined by the characteristic ion peak area external standard method. Results　The detection limits of this method were as below: tetramine' limits were 0.07 µg/ml (blood) and 0.10 µg/ml (urine); fluoroacetamide' limits were 0.01 µg/ml (blood) and 0.02 µg/ml (urine); bromadiolone' limits were 0.06 µg/ml (blood) and 0.04 µg/ml (urine). The method had good reproducibility, and the relative standard deviations were as below: tetramine' deviation was 2.3%-8.1%; tluoroacetamide' deviation was 2.2%-9.9%; bromadiolone's deviation was 2.0%-6.4%. The average recovery rates of tetramine, fluoroacetamide, and bromadiolone were 81.5%-101.8%, 79.5%-103.2%, and 87.6%-98.7%. Conclusion　The method has low detection limits and good precision and recovery, and is suitable for the determination of three rodenticides in whole blood and urine samples of patients with suspected rodenticide poisoning.