液质联机测定尿中拟除虫菊酯类农药代谢物的方法研究

[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0.20 μg/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。

Determination of pyrethroid insecticide metabolites in human urine by liquid chromatography-mass spectrometry

[ Objective] To develop a quantitative method for determination of pyrethroid insecticide metabolites （3 - PBA, Cis - C12C and Trans - C12CA） in human urine by liquid chromatography - tandem quadrupole mass spectrometry. [ Methods ] After acidification and liquid - liquid extraction, the urine samples were analyzed by C18 separation, MS detector and internal standard quantification. [ Results] A good liner relationship was obtained and the correlation coefficient were greater than 0.998. Interday/Intraday relative standard deviation. （ RSD ） and recoveries determined by analysing fortified man- ual synthesis urine were less than 10.0% and 90.0 -110.0% respectively. Limits of detection were 0.20 μg/L. [ Conclusion] As it is easy, convenient and low cost, the method can meet biomonitoring requirements for general or special populations.