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全自动固相萃取-气相色谱串联质谱法测定生活饮用水中9种除草剂残留
引用本文:赵丽,师真,张瑞雨,李文廷,农蕊瑜,李旭. 全自动固相萃取-气相色谱串联质谱法测定生活饮用水中9种除草剂残留[J]. 现代预防医学, 2019, 0(3): 501-505
作者姓名:赵丽  师真  张瑞雨  李文廷  农蕊瑜  李旭
作者单位:昆明市疾病预防控制中心,云南 昆明 650228
摘    要:目的 建立生活饮用水中9种除草剂残留的固相萃取-气相色谱-串联质谱(GC-MS/MS)检测方法。方法 将水样pH调至1.0~2.0,经C18固相萃取柱萃取后,用乙酸乙酯-二氯甲烷(1〖DK〗∶1,v/v)洗脱,洗脱液经氮吹浓缩至近干,并用乙酸乙酯定容后测定。采用DB-35MS 毛细柱分离,选择离子扫描( SIM)模式检测,外标法定量。结果 9种除草剂在0.05~1.0 μg/ml范围内,线性关系良好,方法检出限为0.0001~0.0005 μg /L;平均回收率为72.30 %~105.34 %,相对标准偏差为2.16 %~6.39 %( n =6)。结论 本法操作简便、灵敏、准确,可用于饮用水中多种除草剂残留的同时检测。

关 键 词:生活饮用水  除草剂  气相色谱-串联质谱法  全自动固相萃取

Determination of 9 herbicide residues in water by automatic solid phase extraction combined with GC-MS/MS
ZHAO Li,SHI Zhen,ZHANG Rui-yu,LI Wen-ting,NONG Rui-yu,LI Xu. Determination of 9 herbicide residues in water by automatic solid phase extraction combined with GC-MS/MS[J]. Modern Preventive Medicine, 2019, 0(3): 501-505
Authors:ZHAO Li  SHI Zhen  ZHANG Rui-yu  LI Wen-ting  NONG Rui-yu  LI Xu
Affiliation:Center for Disease Control and Prevention of Kunming,Kunming,Yunnan 650228,China
Abstract:Objective To establish an analytical method for the determination of nine herbicides residues in drinking water by using solid-phase extraction and gas chromatography/mass spectrometry(SPE-GC-MS/MS).Methods The water sample was extracted by C18 solid phase column.The pH of water sample was adjusted to 1.0-2.0 and then eluted by 10.0ml ethyl acetate-dichloromethane(1〖DK〗∶1,v/v)at the speed of 0.5 ml/min.The herbicides were analyzed under selected ion monitoring(SIM)mode and quantified by an external standard method.Results The results showed that the nine herbicides had a good linearity in the range of 0.05-1.0 μg/ml,the average recovery rates measured by standard addition method were in the range of 72.30%-105.34%,and the relative standard deviation( n =6)was in the range of 2.16%-6.39%.The minimum detectable level was 0.0001-0.0005 μg/L.Conclusion The method can be applied to the detection of various herbicide residues in drinking water because it is simple,sensitive and accurate.
Keywords:Drinking water  Herbicides  Gas chromatography-mass spectrometry  Solid phase extraction
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