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

doi:10.7506/spkx1002-6630-20200508-078

食品科学 ›› 2020, Vol. 41 ›› Issue (22): 308-314.doi: 10.7506/spkx1002-6630-20200508-078

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

刘希雅，田春妹，郑鹭飞，钟平胜，张馨方，任佳丽

（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）

出版日期:2020-11-25 发布日期:2020-11-26
基金资助:
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）

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

LIU Xiya, TIAN Chunmei, ZHENG Lufei, ZHONG Pingsheng, ZHANG Xinfang, REN Jiali

(1. Hunan Key Laboratory of Forestry Edible Sources Safety and Processing, Changsha 410004, China; 2. College of Food Science and Engineering, Central South University of Forestry and Technology, Changsha 410004, China; 3. Institute of Quality and Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences, Beijing 100081, China)

Online:2020-11-25 Published:2020-11-26

摘要/Abstract

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1×103～1×108 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=19.77lgN－49.14，检出限为1×102 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。

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

Abstract: In this paper, an electrochemical immunosensor based on magnetic three-dimensional ferroferric oxide/reduced graphene nanocomposite (Fe3O4@3D-RGO) was developed and applied to rapidly detect Mycobacterium tuberculosis H37Ra in milk. Fe3O4@3D-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 H37Ra was detected. The results showed that the sensor displayed a strong linear relationship between the electrode impedance and the logarithmic concentration of M. tuberculosis H37Ra in the range of 1 × 103–1 × 108 CFU/mL. The regression equation was y = 19.77lgN ? 49.14, the limit of detection (LOD) was 1 × 102 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.

Key words: magnetic three-dimensional reduced graphene; modified electrode; Mycobacterium tuberculosis H37Ra; electrochemical immunosensor; rapid detection

中图分类号:

TS207.4

刘希雅，田春妹，郑鹭飞，钟平胜，张馨方，任佳丽. 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[J]. 食品科学, 2020, 41(22): 308-314.

LIU Xiya, TIAN Chunmei, ZHENG Lufei, ZHONG Pingsheng, ZHANG Xinfang, REN Jiali. Preparation of Magnetic Three-Dimensional Reduced Graphene and Its Application in Electrochemical Immunoassay of Mycobacterium tuberculosis H37Ra in Milk[J]. FOOD SCIENCE, 2020, 41(22): 308-314.

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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

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