摘要
本实验通过将5μL MWCNTs-COOH修饰液、Nafion修饰液及其二者的混合修饰液于干净的玻碳电极表面,在红外灯下烤干制得MWCNTs-COOH/GCE修饰电极、Nafion/GCE修饰电极及Nafion/MWCNTs-COOH/GCE修饰电极,采用三电极系统(玻碳电极或修饰电极为工作电极、Ag/Ag Cl为参比电极、铂丝为辅助电极)和快速循环伏安法测定富集在0.2mol/L Li Cl中的孔雀石绿(Malachite Green,MG)浓度,建立快速灵敏检测养殖水中MG含量的方法。MG在Nafion/MWCNTs/GC的循环伏安图表明,在0.57V电位处有良好的氧化峰,未出现还原峰,说明其电化学反应是不可逆氧化还原过程。MG氧化峰电流与其浓度在3×10-7~9×10-6mol/L之间具有良好的线性关系(Ip(μA)=0.207CMG(μmol/L)+3.158,R2=0.985)的优化条件是:修饰材料Nafion与MWC-NTs-COOH之比为1∶1、修饰液用量为5μL、电解质为0.2mol/L Li Cl溶液、表面活性剂CPB的浓度为7×10-5mol/L、MG富集10 min,在此条件下,检测限为6×10-8 mol/L(S/N=3),加标回收率在95.9%~98.7%。使用该方法测定养殖水中MG含量,具有速度快、灵敏度高、稳定性和重复性好的优点。
5μL of MWCNTs-COOH modification solution,Nafion modification solution and their mixed modification liquid were applied on the clean surface of clean glassy carbon electrode and baked under infrared light to obtain MWCNTs-COOH/GCE modified electrode,Nafion/GCE modified electrode and Nafion/MWCNTs-COOH/GCE modified electrode,and thus a rapid and sensitive method for the detection of concentration of malachite green(MG)in 0.2 mol/L Li Cl or detecting MG content in aquaculture water,Nafion/MWCNTs/GC Nano-electrochemical sensor,was established,using a three-electrode system(glassy carbon electrode or modified electrode as working electrode,Ag/Ag Cl as reference electrode,platinum wire as auxiliary electrode)and rapid cyclic voltammetry.The cyclic voltammogram of MG on Nafion/MWCNTs/GC nano-electrochemical sensor showed that a well-defined oxidation peak was observed at 0.57 V but no reduction peak,which indicates that the electrochemical reaction of MG is an irreversible process.The best detection of MG level in aquaculture water by the Nano-electrochemical sensors were observed under the conditions of Nafion∶MWCNTs ratio as 1∶1,the amounts of 5μL,electrolyte solution of 0.2 mol/L Li Cl,concentration of CPB surfactant as 7 x10-5mol/L and enrichment time as 10 min.At the optimum conditions,the oxidation peak currents of MG increased linearly with its concentration in the range of 3×10-7~9×10-6mol/L(Ip(μA)=0.207CMG(μmol/L)+3.158,R2=0.985),with the limit of detection(LOD)as 6×10-8 mol/L(S/N=3).The addition standard recovery of the developed method was varied from 95.9%to 98.7%.The findings indicate that the method here for rapid determination of MG in aquaculture water is more sensitive and accurate compared with the other methods,while it is rapid,convenient,stable and reproducible.
作者
尚晶晶
郝雅茹
李书国
张薇
SHANG Jingjing;HAO Yaru;LI Shuguo;ZHANG Wei(Hebei University of Science and Technology,Shijiazhuang 050018,China;Hebei food inspection and Research Institute,Shijiazhuang 050018,China)
出处
《水产学杂志》
CAS
北大核心
2020年第1期60-66,共7页
Chinese Journal of Fisheries
基金
国家自然科学基金资助项目(20876165)
河北省食品药品安全科技计划项目(ZD2014011)
河北省市场监督管理局科技计划项目(2020ZD15).
关键词
孔雀石绿
农产品安全
纳米传感器
水产养殖
快速检测
malachite green
agricultural product safety
nano-sensor
aquaculture
rapid detection
作者简介
尚晶晶(1992-),女,硕士研究生,研究方向为食品安全快速检测.E-mail:740713569@qq.com;通信作者:李书国(1969-),男,教授,工学博士,研究方向为食品安全快速检测与控制.E-mail:shuguolee@126.com
