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[目的]建立用液相色谱-质谱法测定人尿中3种拟除虫菊酯类农药代谢物(3-PBA、Cis-Cl2CA和Trans-Cl2CA)的定量方法。[方法]样品经酸水解、液液萃取后,用Zorbax SB C18柱分离、大气压化学电离源检测、内标法定量。[结果]方法线性良好,相关系数(R2)>0.998,3个代谢物的日内、日间回收率范围在90.0%～110.0%之间,相对标准偏差(RSD)小于10.0%,检出限为0.20μg/L。[结论]该方法简单、方便、成本低,能满足从普通人群到职业特殊人群的生物监测工作的要求。
[Objective] To establish a method for the quantitative determination of three pyrethroid pesticide metabolites (3-PBA, Cis-Cl2CA and Trans-Cl2CA) in human urine by liquid chromatography-mass spectrometry. [Method] The samples were acid hydrolyzed and liquid - liquid extracted. The samples were separated on a Zorbax SB C18 column and detected by atmospheric pressure chemical ionization source. The samples were quantified by internal standard method. [Result] The method showed a good linearity with a correlation coefficient (R2)> 0.998. The daily and daily recoveries of three metabolites ranged from 90.0% to 110.0% with relative standard deviations (RSDs) less than 10.0%. The detection limits were 0.20 μg / L. [Conclusion] The method is simple, convenient and low cost and can meet the requirements of biological monitoring from general population to occupational special populations.