玉米中乙草胺、莠去津及代谢物残留分析方法研究  

Residue analysis method of acetochlor,atrazine and their metabolites in corn

作　　者：王全胜 吕燕 胡晨雷 吴银良 WANG Quansheng;LYU Yan;HU Chenlei;WU Yinliang(Ningbo Key Laboratory of Testing and Control for Characteristic Agro-Product Quality and Safety,Ningbo Academy of Agricultural Sciences,Ningbo 315040,Zhejiang Province,China)

机构地区：[1]宁波市农业科学研究院宁波市特色农产品质量安全检测与控制重点实验室,浙江宁波315040

出　　处：《农药学学报》2024年第6期1201-1207,共7页Chinese Journal of Pesticide Science

基　　金：宁波市重大科技攻关项目(2021Z056)。

摘　　要：基于改良的QuEChERS法,建立了同时检测玉米中乙草胺(ACE)及其代谢物2-乙基-6-甲基苯胺(EMA)、2-(1-羟乙基)-6-甲基苯胺(HEMA)和莠去津(ATR)及其代谢物脱乙基莠去津(DEA)、脱异丙基莠去津(DIA)、脱乙基脱异丙基莠去津(DACT)、羟基莠去津(HA)的多残留分析方法。目标物经乙腈提取,N-丙基乙二胺(PSA)和无水硫酸镁净化,超高效液相色谱-串联质谱仪(UPLC-MS/MS)检测。结果表明:在0.001~0.02 mg/L范围内,各化合物基质标准工作液的浓度与响应值均呈良好的线性关系,相关系数r≥0.99。在添加水平为0.01~0.5 mg/kg时,各化合物在鲜玉米、籽粒和秸秆中的平均回收率为85%~109%,最大变异系数(RSD)为18%,方法定量限(LOQ)为0.01 mg/kg。方法的正确度、精密度和灵敏度均较好,符合残留分析的要求。Multi-residue analytical method of acetochlor,atrazine and their metabolites(EMA,HEMA,DEA,DIA,DACT,HA)was developed based on the modified QuEChERS.Target compounds were extracted with acetonitrile,purified with PSA and anhydrous magnesium sulfate,and detected with ultra-high performance liquid chromatography-tandem mass spectrometer(UPLC-MS/MS).The results showed that the correlation coefficient(r)was higher than 0.99 within the concentration range of 0.001 to 0.02 mg/L,which indicated a satisfactory linear relationship between the areas and the concentrations of all target compounds.Meanwhile,average recoveries of all compounds in fresh corn,corn kernel and straw were 85%~109%with the relative standard deviation(RSD)≤18%at the spiked level of 0.01 to 0.5 mg/kg.The limit of quantification(LOQ)of the method was 0.01 mg/kg.The results indicated that the trueness,precision and sensitivity of the method met the requirement of residue analysis.

关 键 词：乙草胺 莠去津 代谢物 QUECHERS 超高效液相色谱-串联质谱法 残留分析 

分 类 号：S481.8[农业科学—农药学] TQ450.26[农业科学—植物保护]