摘要
[背景]三嗪类除草剂是我国目前生产应用较多的除草剂之一,其很难被生物降解,具有持续高生态毒性,会对环境产生影响,包括对水生生物的慢性毒性、生态系统中的蓄积以及对人体健康的危害。[目的]将固相萃取法和液相色谱-串联质谱法相结合,建立检测水中莠去津、草净津、异丙甲草胺、草克津、扑草净、西玛津6种三嗪类除草剂的新方法。[方法]优化仪器条件和前处理条件,用Waters Oasis HLB萃取小柱净化,甲醇洗脱,90%甲醇水复溶,超高效液相色谱串联质谱法用电喷雾离子化源正离子模式进行多反应检测模式监测,对质谱测定的目标离子进行选择,外标法定量。应用建立的方法检测4份太湖水样、3份水源水样和10份生活饮用水样。[结果]6种三嗪类除草剂在0-250.0μg·L^(-1)范围内线性关系良好,相关系数均大于0.999,检出限为0.54-1.44μg·L^(-1),定量限为1.8-4.8μg·L^(-1),平均回收率为75.0%-93.3%,精密度为0.6%-5.0%。水源水和生活饮用水中均未检出三嗪类除草剂,某湖水样本中测得草克津质量浓度为0.16-0.17μg·L^(-1),其他5种物质未检出。[结论]方法操作简便,检出限低,灵敏度高,经实际湖水样品测试,可以满足水样中6种除草剂残留的同时分析测定。
[Background] Triazine herbicides are one kind of the most widely used herbicides in China. They are persistent, toxic, and bio-resistant in the environment, including chronic toxicity to aquatic organisms, accumulation in the ecosystem, and harm to human health. [Objective] The methodological research is conducted to establish a method for determination of six triazine herbicides, including atrazine, fortrol, metolachlor, metribuzin, prometryn, and simazine, in water by solid phase extraction(SPE) coupled with liquid chromatography tandem mass spectrometry(LC-MS/MS). [Methods] The instrument conditions and pre-treatment conditions were optimized. Samples were applied to Waters Oasis HLB extraction cartridges, eluted with methanol, and dissolved in 90% methanol. Ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS) in multiple reaction monitoring mode with electrospray ionization source by positive ion mode was used to select target ion pairs for determination. The external standard method was also used for quantitative determination. Four samples of Taihu Lake, three samples of source water, and ten samples of drinking water were detected by the established method.[Results] All the six triazine herbicides had good linear relationships within the range of 0-250.0 μg·L^(-1), and the correlation coefficients were all greater than 0.999. The detection limits were 0.54-1.44 μg·L^(-1), the quantification limits were 1.8-4.8 μg·L^(-1), the average recovery rates were 75.0%-93.3%, and precision ranged from 0.6%-5.0%. Triazine herbicides were not detected in source water and drinking water. The concentration of metribuzin in water samples of a lake was 0.16-0.17 μg·L^(-1), and the other five analytes were not detected. [Conclusion] The method is simple to operate, with a low detection limit and a high sensitivity, and can meet the requirements of simultaneous determination of selected six herbicide residues in lake water samples.
作者
吴宇伉
徐银菊
王晓嫚
徐志飞
梅勇
WU Yukang;XU Yinju;WANG Xiaoman;XU Zhifei;MEI Yong(Wuxi Center for Disease Control and Prevention(The Affiliated Wuxi Center for Disease Control and Prevention of Nanjing Medical University),WuXiz Jiangsu 214023,China;School of Public Health,School of Medicine,Wuhan University of Scienee and Technology,Wuhan,Hubei 430065,China;Key Laboratory of Occupational Hazards Identification and Control in Hubei Province,Wuhan University of Scienee and Technology,Wuhan,Hubei 430065,China)
出处
《环境与职业医学》
CAS
CSCD
北大核心
2021年第6期654-659,共6页
Journal of Environmental and Occupational Medicine
基金
江南大学公共卫生研究中心青年项目(JUPH201843)。
关键词
固相萃取
液相色谱串联质谱法
水
三嗪类除草剂
solid phase extraction
liquid chromatography tandem mass spectrometry
water
triazine herbicides
