摘要
建立全自动固相萃取-气相色谱质谱法监测地表水中的5种有机磷类(对硫磷、甲基对硫磷、马拉硫磷、内吸磷、乐果)农药残留量的检测方法。采用全自动固相萃取技术,选择HLB固相萃取柱对地表水样进行富集和净化;采用多反应监测模式(MRM)经气相色谱质谱联用仪(GC-MS)对样品进行测定,外标法定量。5种有机磷类农药残留量的质量浓度在0.02~2.0μg/mL范围内线性关系良好,线性相关系数均大于0.995,检出限如下:对硫磷:0.014μg/mL、甲基对硫磷:0.010μg/mL、马拉硫磷:0.011μg/mL、内吸磷:0.018μg/mL、乐果:0.008μg/mL。该方法的平均回收率在82.7%~94.8%之间,重复性与精密度测定结果的相对标准偏差均小于5.0%(n=6)。该方法灵敏度与准确度高,自动化程度高,适用于地表水中有机磷类农药残留的监测。
To establish automatic solid phase extraction(SPE)-GC/MS method for determination of 5 organophosphorus(parathion,parathion-methyl,malathion,demeton,dimethoate)pesticides residues in surface water.Using automatic solid phase extraction technology,HLB solid phase extraction column was selected to enich and purify samples.Samples were analyzed by GC/MS by multi-reaction monitoring(MRM).External standard method was selected to quantify pesticides.The concentration of 5 organophosphorus pesticides residues had good linear relationships with its chromatographic peak area in the range of 0.02-2.0μg/mL,with correlation coefficients were all above 0.995.Detection limits were as follows:parathion 0.014μg/mL,parathion-methyl 0.010μg/mL,malathion 0.011μg/mL,demeton 0.018μg/mL,dimethoate 0.008μg/mL.The average recoveries of this method were ranged from 82.7%-94.8%.The results of RSD of reproducibility and precision were all below 5.0%(n=6).The method has high sensitivity and accuracy,with high level automation,and is suitable for the detection of organophosphorus pesticide residues in surface water.
作者
安静
AN Jing(Haidong City Environmental Monitoring Station,Haidong 810699,China)
出处
《中国测试》
CAS
北大核心
2019年第11期61-65,共5页
China Measurement & Test
