大体积固相萃取GC—MS／MS测定水中莠去津的方法研究与应急检测应用  

Study on determination method of atrazine in water by large volume solid phase extraction GC-MS/MS and its application on emergency inspection

作　　者：杜利敏[1] 王彦平[2] 张瑞路 守栋 王龑[1] 

机构地区：[1]郑州市疾病预防控制中心,450007 [2]河南农业职业学院,郑州451450

出　　处：《国际医药卫生导报》2016年第16期2580-2584,共5页International Medicine and Health Guidance News

摘　　要：目的建立生活饮用水及其水源水中莠去津的气相色谱一串联质谱（GC—MS／MS）测定方法。方法选用C18柱采用大体积固相萃取1L水样，浓缩为1ml，溶剂为乙酸乙酯，比较GC—MS／MS在全扫（SCAN）、选择离子扫描（SIM）和多离子反应监测（MRM）三种模式下对水体中莠去津农药残留的定性与定量效果。结果在MRM模式下，莠去津溶液在0．001～5．00μg／ml范围内呈现良好的线性关系，方法的检出限为0．0005μg／L。该方法RSD=6．3％，回收率为88．0％～96．5％，检测效果最好。结论所建立的GC—MS／MS—MRM测定莠去津的方法灵敏度高，特异性好，检出限低，适合生活饮用水及其水源水中痕量莠去津含量的准确测定。Objective To establish the determination method of atrazine in drinking water and source water using gas chromatography-tandem mass spectrometry （GC-MS/MS）. Methods Ethyl acetate was used as solvent to condense 1 L water sample to 1 ml by large volume solid phase extraction with C18 columns. Qualitative and quantitative analyzed the sample in three modes of full scan （sweep）, selective ion scan （SIM）, and multiple reaction monitoring（MRM） in GC-MS/MS. Results In MRM mode, atrazine had good favourable linear correlation when the concentration was 0.001 0-5.000 0 μg/ml and the detection limit of the sample was 0.0005 μg/L. The correlation of instrument response r=0.999 7, RSD=6.3%, with a recovery rate of 88.0%, 96.5%. Conclusion The method established to determin atrazine by GC-MS/MS-MRM has high sensitivity, specificity, and low detection limit. This method is suitable for the accurate determination of the content of trace atrazine in drinking water and waterheads.

关 键 词：大体积固相萃取 气相色谱-串联质谱仪 多反应离子监测 莠去津 

分 类 号：R282.71[医药卫生—中药学]