毛磊红1，杨宏伟2，李殷3
（1 上海康识食品科技有限公司，上海 201103；
2 清华苏州环境创新研究院，苏州 215163；
3 清华大学深圳研究生院，深圳 518055）
摘要：目前国标中对新型农药的检测方法存在前处理较为繁琐，使用大量有机溶剂，检测限较高等问题，而SPELC-MS/MS 检测方法具有前处理有机溶剂消耗较少，过程简单且检测限更低的优点。因此本研究以目前使用较为普遍的稻瘟灵、仲丁威、吡虫啉、甲草胺和西玛津这五种农药为研究对象，通过农药残留检测标准曲线和方法检出限对固相萃取-液相-二级质谱（SPE-LC-MS/MS）方法性能进行评价，最终建立五种农药相应的SPE-LC-MS/MS 检测方法，并利用此方法对水源水和水厂水进行调研，进一步研究水处理工艺对这五种农药的去除情况。结果表明SPE-LC-MS/MS 检测方法可以满足五种农药在水源和饮用水中的检测需求。淮河流域某水源和珠江流域某水源及其沿岸水厂的水源水中稻瘟灵、甲草胺和西玛津是检出浓度较高的农药，最高分别可达到135.4、41.1 和41.5ng/L。水厂处理工艺对稻瘟灵去除效果较好，其中碳滤工艺基本可以将其完全去除，而对吡虫啉则基本无去除效果。纳滤工艺对农药的截留效果较好，对稻瘟灵、吡虫啉、甲草胺和西玛津去除率分别为82.2%、27.4%、89.0%和66.8%。研究结果为农药的检测方法和去除方法提供了参考，膜过滤、臭氧-碳滤等深度处理技术与传统处理工艺相结合在水处理方面对农药有较好的去除效果，有着一定的应用潜力与价值。
关键词：农药；固相萃取-液相-二级质谱法（SPE-LC-MS/MS）；水源水；水厂
Establishment of Pesticide SPE-LC-MS/MS Detection Method and Its Removal Effectin Water Treatment Process
MAO Lei-hong1，YANG Hong-wei2，LI Yin3
（1 Shanghai Kangshi Food Technology Co.，Ltd，Shanghai 201103，China；
2 Tsinghua Suzhou Institute of Environmental Innovation，Suzhou 215000，China；
3 Shenzhen Graduate School of Tsinghua University，Shenzhen 515100，China）
Abstract: At present， the detection method of new pesticides in the national standard has problems such ascumbersome pretreatment，the use of a large number of organic solvents，and the high detection limit，while thesolid phase extraction cartridges- liquid chromatography- secondary mass spectrometry （SPE- LC- MS/MS） detectionmethod has the advantages of less consumption of pretreatment organic solvent，simple process and lower detectionlimit. Therefore，in this study，the five pesticides commonly used in the study were taken as the research objects，namely isoprothiolane，fenobucarb，imidacloprid，alachlor and simazine，and the performance of the solid- phaseextraction-liquid phase-secondary mass spectrometry（SPE-LC-MS/MS）method was evaluated through the standard curve of pesticide residue detection and the detection limit of the method，and the corresponding SPE-LC-MS/MSdetection method for five pesticides was finally established. This method is also used to investigate the source waterand water plant water，and further study the removal of these five pesticides by water treatment process. The resultsshowed that the SPE-LC-MS/MS detection method can meet the detection needs of five pesticides in water sourcesand drinking water. The water of a water source in the Huaihe River Basin and a water source in the Pearl RiverBasin and its coastal water plants were pesticides with high concentrations of isoprothiolane，alachlor and simazine，which could reach 135.4，41.1 and 41.5ng/L，respectively. The treatment process of the water plant has a good effecton the removal of isoprothiolane，among which the carbon filtration process can basically remove it completely，while the imidacloprid has basically no removal effect. The nanofiltration process had a good effect on theinterception of pesticides，and the removal rates of isoprothiolane，imidacloprid，alachlor and simazine were 82.2%，27.4%，89.0% and 66.8%，respectively. The research results provide a reference for the detection methods andremoval methods of pesticides，and the combination of advanced treatment technologies such as membrane filtrationand ozone- carbon filtration with traditional treatment processes has a good removal effect on pesticides in watertreatment，and has certain application potential and value.
Key words: pesticide；solid phase extraction-liquid phase-secondary mass spectrometry（SPE-LC-MS/MS）；sourcewater；water plants
中图分类号：TS275.1 文献标志码：A 文章编号：1007-7871（2023）02-0029-08
2023，Vol.26，No.2