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  

Determination of Pesticide Residues of Parathion-methyl,Parathion, Carbaryl and Metolcarb by HPCE with Amperometric Detection

作　　者：费新平[1] 王立世[1] 张水锋[1] 杨晓云[2] 

机构地区：[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

出　　处：《分析测试学报》2004年第5期70-73,共4页Journal of Instrumental Analysis

基　　金：国家自然科学基金面上项目(批准号20005003)

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。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、α_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 ,α_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)。The determination of parathion,parathion_methyl,metolcarb and carbaryl residues byhigh_perˉformance capillary electrophoresis with amperometric detection is reported.The pesticides were hydrolyzed in alkalescentaqueous solutions,resultinginthe formation of m_methylphenol,α_naphthol and p_nitropheˉnol,which were determined amperometrically after capillary electrophoretic separation.A series of factors affecting pesticide hydrolysis and capillary separation were studied and optimized.The suitable conditions are as follows:potassiumdihydrogen phosphate buffer concentration of5mmol/L,buffer pH10.0,separaˉtion potential20.0kV,workingelectrode potential1.0V(vs.SCE),NaOHconcentration for alkaline hyˉdrolysis by1.0mol/L,hydrolysis temperature-boiling water bath,and hydrolysis duration by15min.Under these conditions,baseline separation of mixed standard phenol samples was achieved within15min.The same linear range of0.05～10mg/Lwas obtained for m_methylphenolα_naphthol and p_nitroˉphenol,and their detection limits(S/N=3)were found to be0.04,0.02and0.03mg/L,respectively.Thus,metolcarb,carbaryl and parathion can be determined indirectly with recovery of91%,94%and101%,and RSD of2.5%,2.2%and3.3%,respectively.The technique was successively applied to the rapid determination of the pesticide residues of metolcarb,carbaryl,parathion and parathion_methyl in vegetables and fruits.

关 键 词：毛细管电泳 安培检测 酚类 农药残留 

分 类 号：O657.8[理学—分析化学] S481.8[理学—化学]