QuEChERS-高效液相色谱-串联质谱法同时测定柿子中螺虫乙酯及其四种代谢物残留  

QuEChERS-High-performance Liquid Chromatography Tandem Mass Spectrometry for the Simultaneous Determination of the Residues of Spirotetramat and Its 4 Metabolites in Diospyros Kaki L.f.

作　　者：陈培玉 刘俊辉[2] 刘丹黎[1] 吴绪金 安莉 李萌 白乐高[1] Chen Peiyu;Liu Junhui;Liu Danli;Wu Xujin;An Li;Li Meng;Bai Legao(Base management center of Henan Academy of Agricultural Sciences,Zhengzhou Henan 450002,China;Henan University of Animal Husbandry and Economy,Zhengzhou Henan 450002,China;Institute of Quality Standard and Testing Technology for Agro-products,Henan Academy of Agricultural Sciences,Zhengzhou Henan 450002,China)

机构地区：[1]河南省农业科学院基地管理中心,河南郑州450002 [2]河南牧业经济学院,河南郑州450002 [3]河南省农业科学院农业质量标准与检测技术研究所,河南郑州450002

出　　处：《农药科学与管理》2022年第10期59-66,共8页Pesticide Science and Administration

基　　金：河南省农业科学院科技创新团队(2022TD20);河南省农业科学院自主创新项目(2022ZC55);河南省农业科学院科技成果示范推广项目(2021FZ07)。

摘　　要：建立柿子中螺虫乙酯及其4种代谢物残留量的QuEChERS前处理方法,高效液相色谱-三重四级杆串联质谱仪器检测方法。样品经乙腈涡旋振荡提取,氯化钠盐析,GCB(石墨化碳黑)、PSA(N-丙基乙二胺)固相萃取材料净化,在MRM模式下,高效液相色谱-三重四级杆串联质谱法检测,基质匹配标准溶液的外标法定量。螺虫乙酯及其4种代谢产物质量浓度与对应峰面积在0.005~0.500mg/L范围内呈良好的线性关系,最低检测浓度为0.01 mg/kg,决定系数R 2在0.9914~0.9997之间。柿子中螺虫乙酯和其4种代谢产物在添加水平为0.01、0.1、10mg/kg时的平均回收率为93%~104%,相对标准偏差为0.8%~4.7%。该方法操作便捷、精准高效、灵敏可靠,适用于同时测定柿子中螺虫乙酯及其代谢产物残留。A method was established for the determination of spirotetramat and its four metabolites residues in Diospyros Kaki L.f,using a QuEChERS pretreatment method and a High-performance liquid chromatography-triple-quadrupole tandem mass spectrometry detection method.The samples were extracted by Acetonitrile Vortex Oscillation,salted out by sodium chloride,purified by solid phase extraction with GCB and PSA,and detected by High-performance liquid chromatography-triple quadrupole tandem mass spectrometry in MRM mode,using the external standard method of matrix matching standard solution.There was a good linear relationship between the mass concentration of spirotetramat and its four metabolites residues and the corresponding peak area in the range of 0.005~0.500 mg/L.The minimum detection concentration was 0.01 mg/kg,and the determination coefficient R 2 was between 0.9914~0.9997.The average recoveries of spirotetramat and its four metabolites residues in Diospyros Kaki L.f were 93%~104%,with the RSD of 0.8%~4.7%when the addition levels were 0.01 mg/kg,0.1 mg/kg and 10 mg/kg,respectively.The method is simple,accurate,efficient,sensitive and reliable enough for the simultaneous determination of spirotetramat and its four metabolites residues in Diospyros Kaki L.f.

关 键 词：螺虫乙酯 代谢物 柿子 残留 

分 类 号：S482.3[农业科学—农药学] S481[农业科学—植物保护]