磁性三维还原石墨烯的制备及其在电化学免疫检测牛乳中结核杆菌H37Ra的应用  

Preparation of Magnetic Three-Dimensional Reduced Graphene and Its Application in Electrochemical Immunoassay of Mycobacterium tuberculosis H37Ra in Milk

作　　者：刘希雅 田春妹 郑鹭飞[3] 钟平胜 张馨方 任佳丽 LIU Xiya;TIAN Chunmei;ZHENG Lufei;ZHONG Pingsheng;ZHANG Xinfang;REN Jiali(Hunan Key Laboratory of Forestry Edible Sources Safety and Processing,Changsha 410004,China;College of Food Science and Engineering,Central South University of Forestry and Technology,Changsha 410004,China;Institute of Quality and Testing Technology for Agro-products,Chinese Academy of Agricultural Sciences,Beijing 100081,China)

机构地区：[1]林产可食资源安全与加工利用湖南省重点实验室,湖南长沙410004 [2]中南林业科技大学食品科学与工程学院,湖南长沙410004 [3]中国农业科学院农业质量标准与检测技术研究所,北京100081

出　　处：《食品科学》2020年第22期308-314,共7页Food Science

基　　金：国家自然科学基金面上项目(31972173);湖南省创新型省份建设专项(2019TP1029);湖南省科技创新计划项目(2018XK2006);长沙市科技计划项目(kq1901143);农业部农产品质量安全风险评估项目(GJFP2019017);湖南省林业科技创新专项(XLK201904)。

摘　　要：研制基于四氧化三铁/三维还原氧化石墨烯(ferroferric oxide/three-dimensional reduced graphene oxide,Fe3O4@3D-RGO)复合修饰材料的电化学免疫传感器,并将其应用于牛乳中结核杆菌H37Ra的快速检测。采用水热一步还原法合成了Fe3O4@3D-RGO复合材料,并利用扫描电镜、电子能谱和拉曼光谱对材料进行表征;采用75%的乙醇和0.1%Nafion溶液作为分散体系制备了修饰电极,运用交流阻抗法(electrochemical impedance spectroscopy,EIS)对其电化学性能进行探讨,在最优条件下采用EIS法进行结核杆菌H37Ra的检测。结果显示,H37Ra浓度在1×10^3~1×10^8 CFU/mL范围内,电极阻抗与浓度的对数呈现较强的线性关系,回归方程为y=19.771gN-49.14,检出限为1×10^2 CFU/mL,检测时间15 min。该方法特异性强、重复性和稳定性良好。采用水热一步还原法制备Fe3O4@3D-RGO简便、环保,为便携式电化学免疫传感器的开发提供了技术支撑。In this paper,an electrochemical immunosensor based on magnetic three-dimensional ferroferric oxide/reduced graphene nanocomposite(Fe3 O4@3 D-RGO)was developed and applied to rapidly detect Mycobacterium tuberculosis H37 Ra in milk.Fe3 O4@3 D-RGO was synthesized by a one-step hydrothermal reduction method and then characterized by scanning electron microscopy,electron energy spectroscopy and Raman spectroscopy.A modified electrode was prepared with 75%ethanol and 0.1%Nafion solution as dispersion system.The electrochemical performance was investigated using electrochemical impedance spectroscopy(EIS).Under the optimal conditions,M.tuberculosis H37 Ra was detected.The results showed that the sensor displayed a strong linear relationship between the electrode impedance and the logarithmic concentration of M.tuberculosis H37 Ra in the range of 1×10^3-1×10^8 CFU/mL.The regression equation was y=19.77 lgN-49.14,the limit of detection(LOD)was 1×10^2 CFU/mL and the detection time was as short as 15 min.This method had strong specificity and good repeatability and stability.The one-step hydrothermal reduction method,thanks to its simplicity and environmental friendliness,provides technical support for the development of portable electrochemical immunosensors.

关 键 词：磁性三维还原石墨烯 修饰电极 结核杆菌H37Ra 电化学免疫传感器 快速检测 

分 类 号：TS207.4[轻工技术与工程—食品科学]