黄瓜和土壤中吡唑醚菌酯和霜脲氰同步检测及其降解分析

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1、2622018,Vol.39,No.08食品科学※安全检测黄瓜和土壤中吡唑醚菌酯和霜脲氰同步检测及其降解分析11,*，张 超1111111洪思慧，佘永新，曹晓林，郑鹭飞，王珊珊，金茂俊，邵 华，金 芬，221,*劳水兵，闫飞燕，王 静（1.中国农业科学院农业质量标准与检测技术研究所，北京100081；2.广西壮族自治区农业科学院农产品质量安全与检测技术研究所，广西南宁530227）摘 要：采用QuEChERS-液相色谱-串联质谱法，建立黄瓜及土壤中吡唑醚菌酯和霜脲氰同步检测方法，研究吡唑醚菌酯·霜脲氰水分散粒剂在黄瓜和土壤中的残留变化及消解动态，

2、旨在评估联合农药的安全性。样品经乙腈提取，N-丙基乙二胺吸附剂和十八烷基键合硅胶吸附剂净化，质谱多反应监测模式扫描。在50～800μg/L之间具有良好的线性关系，r值均大于0.9961，3个质量浓度添加水平下2种农药在黄瓜和土壤中的平均回收率为70.45%～107.08%，定量限均为0.050mg/kg。两年三地的田间实验消解动态表明：以1.5倍高推荐剂量下，吡唑醚菌酯和霜脲氰分别于黄瓜上施药1、7d后，土壤上施药7、1d后残留量小于定量限；当该制剂以推荐剂量在黄瓜上施药3次，施药间隔7d时，吡唑醚菌酯和霜脲氰在黄瓜中的最高残留量分别为0.090

3、mg/kg和0.060mg/kg，远低于我国规定的最大残留限量0.5mg/kg，推荐采收安全间隔期为3d。关键词：吡唑醚菌酯；霜脲氰；黄瓜；土壤；QuEChERS；高效液相色谱-串联质谱法；残留；消解动态SimultaneousDetectionandDegradationofPyraclostrobinandCymoxanilinCucumberandSoil11,*,ZHANGChao111HONGSihui,SHEYongxin,CAOXiaolin,ZHENGLufei,1111221,*WANGShanshan,JINMaojun,SH

4、AOHua,JINFen,LAOShuibing,YANFeiyan,WANGJing(1.InstituteofQualityStandardandTestingTechnologyforAgro-Products,ChineseAcademyofAgriculturalSciences,Beijing100081,China;2.InstituteofQualityStandardandTestingTechnologyforAgro-Products,GuangxiAcademyofAgriculturalSciences,Nanning5

5、30227,China)Abstract:Inthispaper,amethodforthesimultaneousdetectionofpyraclostrobinandcymoxanilincucumberandsoilwasdevelopedusingthequick,easy,cheap,effective,ruggedandsafe(QuEChERS)methodcoupledwithhighperformanceliquidchromatography-tandemmassspectrometry(HPLC-MS/MS).Thedeg

6、radationkineticsandthefinalresidueofpyraclostrobin-cymoxanilwaterdispersiblegranuleincucumberandsoilwerestudied,aimingtoevaluatethesafetyofthispesticidecombination.Sampleswereextractedwithacetonitrileandtheextractwascleanedupwithprimarysecondaryamine(PSA)andC18beforebeinganal

7、yzedbymassspectrometryinthemultiple-reactionmonitoring(MRM)mode.There2wasagoodlinearrelationshipwithintheconcentrationrangeof50–800μg/Lwithcorrelationcoefficients(R)greaterthan0.9961.Theaveragerecoveriesoftwopesticidesincucumberandsoilwere70.45%–107.08%atthreespikedconcentrat

8、ions.Thelimitofquantification(LOQ)was0.050mg/kgforboth.Two-yearfieldex