超高效液相色谱-串联质谱法测定水中甲拌磷及其代谢物残留量  

Determination of phorate and its metabolites residues in water by ultra performance liquid chromatography tandem mass spectrometry

作　　者：陈永平 付志茹 韩现芹 时文博 高丽娜 包艳[2] CHEN Yong-Ping;FU Zhi-Ru;HAN Xian-Qin;SHI Wen-Bo;GAO Li-Na;BAO Yan(Tianjin Agricultural Ecological Environment Monitoring and Agricultural Product Quality Testing Center,Tianjin 300221,China;Qingdao Institute of Bioenergy and Bioprocess Technology,Chinese Academy of Sciences,Qingdao 266101,China)

机构地区：[1]天津市农业生态环境监测与农产品质量检测中心,天津300221 [2]中国科学院青岛生物能源与过程研究所,青岛266101

出　　处：《食品安全质量检测学报》2021年第1期168-174,共7页Journal of Food Safety and Quality

基　　金：天津市科技计划项目(17YFNZNC00110)。

摘　　要：目的建立超高效液相色谱-串联质谱法测定水中甲拌磷及其代谢物残留量。方法样品经二氯甲烷提取净化后,采用液相色谱-串联质谱法测定,外标法定量。结果甲拌磷、甲拌磷砜、甲拌磷亚砜在质量浓度2~100 ng/mL范围内线性关系良好(r≥0.9996),检出限为2 ng/L,定量限为5 ng/L。在5、10、50 ng/L加标水平下,加标回收率为73.2%~85.9%,相对标准偏差为1.5%-6.2%。结论本方法适用于检测水中甲拌磷及其代谢物残留量,为水产养殖水中甲拌磷及其代谢物污染源排查及生态环境评价提供可靠的检测技术手段。Objective To establish an analytical method for the determination of phorate and its metabolites in water by ultra performance liquid chromatography-mass spectrometry.Methods The samples were extracted and purified by dichloromethane,then determined by ultra performance liquid chromatography tandem-mass spectrometry,and quantified by external standard method.Results Methylphosphorous sulfoxide,methylph osphorous sulfoxide and methylphosphorous sulfoxide had good linear relationships within the mass concentration range of 2-100 ng/mL(r≥0.9996).The limit of detection was 2 ng/L and the limit of quantitative was 5 ng/L.The recoveries were 73.2%-85.9%,and the relative standard deviations were 1.5%-6.2%at levels of 5,10 and 50 ng/mL.Conclusion This method is suitable for detecting the residues of methyl phosphorus and its metabolites in water.It can provide a reliable detecting technique for the pollution sources of phosphorus and its metabolites in aquaculture water and the ecological environment evaluation.

关 键 词：水 超高效液相色谱-质谱法 甲拌磷及其代谢物 残留量 

分 类 号：X832[环境科学与工程—环境工程] O657.63[理学—分析化学]