Fe-Co尖晶石型复合氧化物电催化检测牛奶中过氧化氢  

Electrocatalytic determination of hydrogen peroxide in milk with Fe-Co spinel composite oxides

作　　者：马懿 陈晓姣 刘自山 伍辉祥 MA Yi;CHEN Xiaojiao;LIU Zishan;WU Huixiang(College of Biological Engineering,Sichuan University of Science and Engineering,Yibin 644005,China;Guangdong Institute of Product Quality Supervision and Inspection Light Industry Textile Garment Testing Department,Guangzhou 510670,China)

机构地区：[1]四川轻化工大学生物工程学院,宜宾644005 [2]广东产品质量监督检验研究院轻工纺织服装检测部,广州510670

出　　处：《农业工程学报》2023年第3期260-264,共5页Transactions of the Chinese Society of Agricultural Engineering

基　　金：四川省自然基金项目(2020YJ0402);2020年五粮液股份公司-四川轻化工大学产学研合作项目(CXY2020ZR004)。

摘　　要：为了高效检测牛奶中H_(2)O_(2)含量,该研究提出了一种基于ZnFeCoO_(4)催化还原H_(2)O_(2)的非酶电化学传感器。首先,通过溶胶-凝胶燃烧法合成ZnCo_(2)O_(4),再利用Fe部分取代Co合成ZnFeCoO_(4)。采用透射电子显微镜、X射线衍射及X射线光电子能谱对催化剂的晶体结构和形貌进行表征,并采用循环伏安法对该电极的电化学性能进行研究。结果表明:ZnFeCoO_(4)具有较好的晶型,基于ZnFeCoO_(4)的电化学传感器对H_(2)O_(2)有良好的电催化性能,检测限为0.5μmol/L;过氧化氢浓度在0.5~2.5 mmol/L范围内与还原峰电流呈线性关系,决定系数为0.989。此外,传感器对H_(2)O_(2)具有优异重现性和选择性。在实际牛奶样品的加标试验中回收率达到98.60%~101.23%。研究可为液态食品中检测H_(2)O_(2)提供重要的应用参考。The objective of this study was to develop an efficient non-enzymatic electrochemical sensor for H_(2)O_(2)detection in milk using the catalytic reduction of H_(2)O_(2)on ZnFeCoO_(4).Firstly,ZnFeCoO_(4)derived from ZnCo_(2)O_(4)by the partial substitution of Co with Fe was synthesized via sol-gel combustion.In ZnCo_(2)O_(4),1 mmol Zn(NO3)2·6H2O and 2 mmol of Co(NO3)2·6H2O were dissolved in a nitric acid solution(2 mL of nitric acid,and 30ml of distilled water).The sticky gel was subsequently obtained by adding 15 mmol citric acid and stirring for 5 h in the oil bath at 90℃.After that,the gel was placed in a 170℃oven(10℃/min heating rate)for 12 h.Then,the moisture-removed gel was crushed with a mortar.Finally,the powder was calcined in a 600℃tubular furnace(5℃/min heating rate)for 6 hours to obtain the spinel phase ZnCo_(2)O_(4)powder.The preparation process of ZnFeCoO_(4)was consistent with that of ZnCo_(2)O_(4).The only difference was that the 2 mmol of Co(NO3)2·6H2O was replaced with 2 mmol of Fe(NO3)2·6H2O.Transmission electron microscopy,X-ray diffraction,and X-ray photoelectron spectroscopy were used to characterize the crystal structure and morphology of the catalyst,while cyclic voltammetry(CV)was used to study the electrochemical performance of the electrode.In order to verify the effectiveness of the ZnFeCoO_(4)electrode in detecting H_(2)O_(2)content in milk,the milk from the local supermarket was centrifuged and 1 mL supernatant was dissolved in 10 mL PBS(pH value 7.4).Standard addition was used for the recovery experiment.The results showed that a similar morphology was obtained after the partial or complete replacement of Co with Fe.ZnFeCoO_(4)presented a better crystal shape and high consistency with the standard database card JCPDS No.23-1390.The mass ratios of Zn,Co,and Fe were measured as 31.46%,35.77%,and 27.15%,respectively,and the molar ratio was about 1:1.2:1,which roughly met the chemical expression of the compound.The XRD patterns of ZnCo_(2)O_(4)and ZnFeCoO_(4)showed that the

关 键 词：电化学传感器 检测 过氧化氢 ZnFeCoO4 牛奶 

分 类 号：TS207.3[轻工技术与工程—食品科学]