γ-CD/g-C_(3)N_(4)修饰电极伏安法检测磺胺二甲基嘧啶  

Detection of sulfamethazine by voltammetry based onγ-CD/g-C_(3)N_(4) nanosheets modified electrode

作　　者：胡华丽 王鑫 艾纪星 周欢喜 张艳[1] 王德响 段禹 任书慧 杜海军[1] HU Huali;WANG Xin;AI Jixing;ZHOU Huanxi;ZHANG Yan;WANG Dexiang;DUAN Yu;REN Shuhui;DU Haijun(School of Chemical Engineering,Guizhou Minzu University,Guiyang 550025,China;School of Mechatronics Engineering,Guizhou Minzu University,Guiyang 550025,China)

机构地区：[1]贵州民族大学化学工程学院,贵阳550025 [2]贵州民族大学机械电子与工程学院,贵阳550025

出　　处：《分析试验室》2023年第5期569-577,共9页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金(81860701,82060714);贵州省高等学校“绿色化学与资源环境创新团队”项目(黔教技[2022]013号);贵州民族大学自然科学基金资助项目(校科字(2019)1号)资助。

摘　　要：采用热聚合法以三聚氰胺为原料制备出块状氮化碳(b-C3N4),通过超声剥离法对b-C_(3)N_(4)进行剥离得到类石墨相氮化碳(g-C3N4),将其与γ-环糊精(γ-CD)复合后得到γ-CD/g-C_(3)N_(4)复合材料。通过滴涂法将复合材料修饰在玻碳电极(GCE)上,构建出灵敏检测磺胺二甲基嘧啶(SM2)的传感器。在优化条件下对SM2进行电化学分析,结果显示SM2在该电极上受吸附控制,电子转移数为2。检测范围为1~150μmol/L和150~750μmol/L,检出限(LOD)为0.79μmol/L。加入50倍K^(+),Ca^(2+),Fe^(3+),Cu^(2+),NH_(4)^(+),SO_(4)^(2-),NO_(3)^(-),盐酸金霉素、维生素、对氨苯甲酸干扰物后电流信号变化较小,相对标准偏差(RSD)为3.5%,将修饰电极存放5 d和10 d后电流信号保留值分别为93%和87%。利用加标回收法测定实际样品纯牛奶中的SM2,回收率为84%~113%,RSD小于5%。Bulk carbon nitride(b-_(3)N_(4))was prepared from melamine by thermal polymerization method.The graphitic carbon nitride(g-_(3)N_(4))was prepared by recombining ultrasonication method,andγ-CD/g-_(3)N_(4) composites were obtained by ultrasonication g-_(3)N_(4) withγ-cyclodextrin(γ-CD).The working electrode of the sensor for sulfamethazine(SM2)detection was decorated by γ-CD/g-_(3)N_(4) on glassy carbon electrode(GCE).Electrochemical analysis of SM2 was performed under optimized conditions,and the results showed that the determination of SM2 on this electrode was controlled by adsorption.The linear range of this method was 1-150μmol/L and 150-750μmol/L with a detection limit of 0.79μmol/L.Results showed that the determination was not interfered after adding 50 times K^(+),Ca^(2+),Fe^(3+),Cu^(2+),NH_(4)^(+),SO_(4)^(2-),NO_(3)^(-),chlortetracycline hydrochloride,vitamins,paraaminobenzoic acid and other interfering substances.In addition,the peak currents retained 93% and 87% of the original response after the electrode was stored for 5 d and 10 d at 5℃,respectively.This method was successfully applied to determine the levels of SM2 in milk samples with good recoveries ranging from 84% to 113% and the relative standard deviations(RSD)was lower than 5%.

关 键 词：磺胺二甲基嘧啶 类石墨相氮化碳 Γ-环糊精 电化学分析 电化学传感器 

分 类 号：O657.1[理学—分析化学]