聚鲁米诺修饰复合电极电化学发光分析法测定豆类样品中钼(Ⅵ)含量  

Electrochemiluminescence Determination of Mo(Ⅵ)Content in Beans Based on Polyluminol Composite Modified Electrode

作　　者：徐艺凤 徐承娥 熊海涛[1] XU Yifeng;XU Cheng’e;XIONG Haitao(School of Chemical and Environmental Sciences,Shaanxi University of Technology,Hanzhong 723001,China)

机构地区：[1]陕西理工大学化学与环境科学学院,陕西汉中723001

出　　处：《食品工业科技》2024年第5期205-211,共7页Science and Technology of Food Industry

基　　金：国家级大学生创新创业训练计划(202110720022);陕西理工大学人才启动项目(SLGRC07)。

摘　　要：本研究基于Mo(Ⅵ)对鲁米诺电还原发光信号的增敏作用,结合石墨烯与带正电荷的纳米金((+)AuNPs)的电信号放大作用,建立了一种灵敏且准确检测豆类种子中Mo(Ⅵ)含量的电化学发光新方法。采用滴涂法先将Nafion-石墨烯修饰于玻碳电极表面,再通过静电组装及电化学聚合技术依次将(+)AuNPs、鲁米诺修饰于电极表面,从而制得Nafion-石墨烯/(+)AuNPs/聚鲁米诺复合修饰电极。通过循环伏安法与电化学发光技术对复合修饰电极进行了初步表征,并对测定Mo(Ⅵ)的实验条件进行了优化。结果表明,在饱和硼砂缓冲溶液、电位扫描速率100 mV/s、富集时间13 min等优化实验条件下,Mo(Ⅵ)浓度在5.0×10^(−9)~1.0×10^(−6)mol/L范围内与复合修饰电极表面增敏的电还原发光信号呈现良好的线性关系,检出限(3σ)与相对标准偏差分别为2.1×10^(−9)mol/L及2.4%(C=1.0×10^(−7)mol/L,n=11)。应用该方法测定了黄豆与绿豆中Mo(Ⅵ)的含量,回收率在91.42%~108.0%之间。该方法简单、经济,有望应用于其它豆类种子中Mo(Ⅵ)含量的准确检测。In this study,based on the sensitization effect of Mo(Ⅵ)on luminol electroreduction luminescence signals,combined with the amplifying effect of graphene and positively charged gold nanoparticle((+)AuNPs),a novel electrochemiluminescence method for sensitive and accurate detection of Mo(Ⅵ)content in legumes seeds was established.The Nafion-graphene/(+)AuNPs/polyluminol composite modified electrode was firstly prepared by the drip coating method,and then(+)AuNPs and luminol were modified on the surface of the Nafion-graphene composite electrode by electrostatic assembly and electrochemical polymerization technology.The composite modified electrode was characterized by cyclic voltammetry and ECL technology,and the experimental conditions for determination of Mo(Ⅵ)were optimized.The results showed that the optimal experimental conditions for the determination of Mo(Ⅵ)were saturated borax buffer solution,potential scanning rate of 100 mV/s and concentrated time of 13 minutes.Under the selected conditions,the concentration of Mo(Ⅵ)was well linear with the enhancement of electroreduction luminous signal in the range of 5.0×10^(−9)~1.0×10^(−6)mol/L.Detection limit of the method and relative standard deviation(RSD)was 2.1×10^(−9)mol/L(3σ,C=1.0×10^(−7)mol/L,n=11)and 2.4%,respectively.This method had been applied to the detection of Mo(Ⅵ)content from soybean and mung beans.The recovery rate was between 91.42%and 108.0%.This proposed method is simple and economical,and is expected to be applied to the accurate determination of Mo(Ⅵ)content in other beans seeds.

关 键 词：聚鲁米诺 电化学聚合 电化学发光 黄豆 绿豆 Mo(Ⅵ) 

分 类 号：TS207.3[轻工技术与工程—食品科学]