摘要
建立液液萃取-气相色谱-质谱法同时测定水中8种酰胺类农药含量。以二氯甲烷-乙酸乙酯(体积比为1∶1)混合溶剂为萃取溶剂,对样品萃取2次,调节溶液pH值为7,NaCl质量浓度为0.03 g/mL,采用选择离子扫描模式检测,内标法定量。8种酰胺类农药的质量浓度在0.1~5.0 mg/L范围内与对应的色谱峰面积具有良好的线性关系,相关系数均不小于0.998。当取样体积为1000 mL时,方法检出限为0.1~0.2μg/L。3个加标水平(0.5、2.0、4.0μg/L)的平均回收率为86.1%~106%,测定结果的相对标准偏差为4.4%~10%(n=6)。该方法可用于水中8种酰胺类农药的同时测定。
A method of liquid-liquid extraction coupled with gas chromatography-mass spectrometry was established for simultaneous determination of eight amide pesticides in water.A mixed solvent of dichloromethane and ethyl acetate(volume ratio 1:1)was used as the extraction solvent,and the sample was extracted twice.The solution pH was adjusted to 7,and the mass concentration of NaCl was set at 0.03 g/mL.Detection was performed in selective ion monitoring mode,and quantification was carried out using the internal standard method.The mass concentrations of the eight amide pesticides had good linear relationship with the corresponding chromatographic peak areas in the range of 0.1-5.0 mg/L,and the correlation coefficients were not less than 0.998.When the sample volume was 1000 mL,the detection limits of the method were 0.1-0.2μg/L.The average recoveries at three spiked levels(0.5,2.0,4.0μg/L)were 86.1%-106%,and the relative standard deviations of the measurement results for six parallel samples were 4.4%-10%.This method can be used for simultaneous determination of eight amide pesticides in water.
作者
曲亚辉
张兆鑫
卢婷婷
曹宁宁
张凯
石勇丽
QU Yahui;ZHANG Zhaoxin;LU Tingting;CAO Ningning;ZHANG Kai;SHI Yongli(Institute of Geological Experiment and Testing,Henan Academy of Geology,Key Laboratory of Water and Soil Resources Protection and Rehabilitation in the Middle and Lower Reaches of the Yellow River Basin,Ministry of Natural Resources,Henan Province Natural Resources Science and Technology Innovation Center(Research on Water and Soil Ecological Restoration and Management),Zhengzhou 450000,China;School of Chemical Engineering,Zhengzhou University,Zhengzhou 450000,China)
出处
《化学分析计量》
2026年第1期94-99,共6页
Chemical Analysis And Meterage
基金
河南省自然资源“揭榜挂帅”科研项目(2024-7)
河南省科技攻关项目(No.252102320095)
河南省科技攻关项目(No.252102320091)
河南省地质研究院地质科技攻关“揭榜挂帅”项目(2025-903-XM08)。
关键词
液液萃取
气相色谱-质谱法
酰胺类农药
liquid-liquid extraction
gas chromatography-mass spectrometry
amide pesticides
