尿中8种氨基甲酸酯类农药快速测定的液相色谱-串联质谱法  

Rapid determination of 8 urinary carbamate pesticides by liquid chromatography-tandem mass spectrometry

作　　者：刘华良[1] 王媛[1] 朱宝立[1] 

机构地区：[1]江苏省疾病预防控制中心,南京210009

出　　处：《中华劳动卫生职业病杂志》2015年第11期857-859,共3页Chinese Journal of Industrial Hygiene and Occupational Diseases

摘　　要：目的 建立尿中8种氨基甲酸酯类农药同时测定的方法.方法 尿样用乙腈沉淀蛋白后,用液相色谱-串联质谱法进行测定,外标法定量,其中色谱柱采用C18超高效液相色谱柱,流动相为甲醇与乙酸铵溶液梯度淋洗,质谱采集方式为多反应监测.结果 样品中氨基甲酸酯类农药的线性范围为20-800 μg/L,当添加浓度为20、200、800 μg/L时,回收率为61.0％-121％,相对标准偏差为1.7％-5.5％.结论 该检测方法各项指标均符合GBZT 210.5-2008《职业卫生标准制定指南第5部分：生物材料中化学物质测定方法》的要求,适用于中毒患者尿中8种氨基甲酸酯类农药的同时检测。Objective To establish a method for simultaneously determining the urinary concentrations of 8 carbamate pesticides.Methods After being purified by acetonitrile precipitation,urine samples were transferred to a liquid chromatography-tandem mass spectrometry system,and the concentrations of 8 carbamate pesticides were determined by external standard method.A C18 column was used for ultra-high-performance liquid chromatography;methanol/ammonium acetate solution was used as the mobile phase for gradient elution;the mass spectrometer was operated in a multi-reaction monitoring mode.Results The calibration curves were linear when the urinary concentrations of these carbamate pesticides were 20～800 μg/L,and the recovery rates were 61.0%～121% at spiked levels of 20,200 and 800 μg/L,with a relative standard deviation of 1.7%～5.5%.Conclusion This determination method meets the Guide for establishing occupational health standards-part 5：Determination methods of chemicals in biological materials,and can be used for simultaneous determination of 8 carbamate pesticides in the urine of poisoning patients.

关 键 词：农药 除莠剂 氨基甲酸酯 色谱法 高压液相 光谱分析 

分 类 号：R139.2[医药卫生—劳动卫生]