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1、第23卷第5期分析测试学报Vol.23No.52004年9月FENXICESHIXUEBAO(JournalofInstrumentalAnalysis)70~73毛细管电泳-安培检测法对甲基对硫磷、对硫磷、西维因和速灭威农药残留的测定研究1112费新平,王立世,张水锋,杨晓云(1.华南理工大学应用化学系,广东广州510641;2.华南农业大学资源环境学院,广东广州510642)摘要:采用高效毛细管电泳-安培检测法对农药甲基对硫磷、对硫磷、西维因和速灭威水解产物酚类进行了测定研究,考察了影响水解和毛细管分离的各种因素:磷酸盐缓冲溶液的浓度、体系的pH值、分离高压、检测电位等。
2、结果表明:在优化的实验条件下,标准样品15min内实现了基线分离,线性范围(mg/L):间_甲酚、A_萘酚和对硝基苯酚均为0.05~10,信噪比为3时,测定检出限(mg/L):间_甲酚0.04,A_萘酚0.02,对硝基苯酚0.03;对硫磷、速灭威和西维因回收率分别为91%,94%和101%,相对标准偏差分别为3.3%、2.5%和2.2%(n=6)。可用于对所选该类农药残留的快速测定。关键词:毛细管电泳;安培检测;酚类;农药残留中图分类号:O657.8;S481.8文献标识码:A文章编号:1004-4957(2004)05-0070-04DeterminationofPesti
3、cideResiduesofParathion_methyl,Parathion,CarbarylandMetolcarbbyHPCEwithAmperometricDetection1112FEIXin_ping,WANGLi_shi,ZHANGShui_feng,YANGXiao_yun(1.DepartmentofChemistry,SouthChinaUniversityofTechnology,Guangzhou510641,China;2.CollegeofResourcesandEnvironment,SouthChinaAgricultureUniversit
4、y,Guangzhou510642,China)Abstract:Thedeterminationofparathion,parathion_methyl,metolcarbandcarbarylresiduesbyhigh_pe-rformancecapillaryelectrophoresiswithamperometricdetectionisreported.Thepesticideswerehydrolyzedinalkalescentaqueoussolutions,resultingintheformationofm_methylphenol,A_naphtho
5、landp_nitrophe-nol,whichweredeterminedamperometricallyaftercapillaryelectrophoreticseparation.Aseriesoffactorsaffectingpesticidehydrolysisandcapillaryseparationwerestudiedandoptimized.Thesuitableconditionsareasfollows:potassiumdihydrogenphosphatebufferconcentrationof5mmol/L,bufferpH10.0,sep
6、ara-tionpotential20.0kV,workingelectrodepotential1.0V(vs.SCE),NaOHconcentrationforalkalinehy-drolysisby1.0mol/L,hydrolysistemperature-boilingwaterbath,andhydrolysisdurationby15min.Undertheseconditions,baselineseparationofmixedstandardphenolsampleswasachievedwithin15min.Thesamelinearrangeof0
7、.05~10mg/Lwasobtainedform_methylphenolA_naphtholandp_nitro-phenol,andtheirdetectionlimits(S/N=3)werefoundtobe0.04,0.02and0.03mg/L,respectively.Thus,metolcarb,carbarylandparathioncanbedeterminedindirectlywithrecoveryof91%,94%and101%,andRSDof2.5%,2.2%and3.
