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作 者:司晓晶 杨力赫 薛天豪 李薇 韩梅 SI Xiaojing;YANG Lihe;XUE Tianhao;LI Wei;HAN Mei(Department of Food Science,Shanghai Business School,Shanghai 200235,China)
出 处:《分析试验室》2024年第7期933-938,共6页Chinese Journal of Analysis Laboratory
基 金:国家自然科学基金(32102007);上海商学院教学质量建设项目(2022-XJKCSZ-05,2023-XJJK-18)资助。
摘 要:建立了基于Ni-Mo双金属氧化物复合纳米材料(NiMoO_(4)/CNF)的电化学传感平台快速检测保健品中褪黑素含量的方法。使用六水合硝酸镍(Ni(NO_(3))_(2)·6H_(2)O),钼酸铵((NH4)2MoO4)和碳纳米纤维(CNF),一步水热法合成了NiMoO_(4)/CNF,将其修饰到玻碳电极(GCE)上制成NiMoO_(4)/CNF/GCE。通过电子扫描电镜、X射线能谱仪、傅里叶红外光谱仪、X射线衍射仪表征NiMoO_(4)/CNF复合材料的形貌、元素组成和基团作用,使用电化学阻抗、循环伏安法和微分脉冲伏安法研究褪黑素在NiMoO_(4)/CNF/GCE上的电化学行为。结果表明,在0.1 mol/L pH 7.5的磷酸盐(PBS)缓冲溶液中,褪黑素浓度与峰电流值线性关系良好,线性方程为I(μmol/L)=0.0195c+1.9971,线性范围为0.5~200μmol/L,检出限为0.17μmol/L。使用该电化学传感器测得某保健品中褪黑素的平均含量为9.43μmol/L,回收率为106.3%,相对标准偏差(RSD)为2.3%。An electrochemical sensing platform based on Ni-Mo bimetal oxide composite(NiMoO_(4)/CNF)was fabricated for rapid detection of melatonin in health products.Ni(NO_(3))_(2)•6H_(2)O,(NH_(4))_(2)MoO_(4) and carbon nanofibers(CNF)were used to produce NiMoO_(4)/CNF composite by one-step hydrothermal method,and then NiMoO_(4)/CNF were drip-coated on glass carbon electrode(GCE)to make Ni-Mo bimetal oxide electrochemical sensor(NiMoO_(4)/CNF/GCE).The morphology,elemental composition and group interaction of the NiMoO_(4)/CNF composite were characterized by electron scanning electron microscopy,X-ray energy spectrometer,Fourier transform infrared spectroscopy and X-ray diffraction.Electrochemical impedance spectroscopy,cyclic voltammetry and differential pulse voltammetry were used to study the electrochemical behavior of melatonin on the NiMoO_(4)/CNF/GCE.The results showed that melatonin had a good linear relationship in 0.1 mol/L phosphate buffer solution(PBS)with pH 7.5 in the range of 0.5-200μmol/L,and the correlation equation was I(μmol/L)=0.0195c+1.9971,with the correlation coefficient(R2)of 0.9923.The detection limit was 0.17μmol/L.The average content of melatonin in a health product detected by this electrochemical sensor was 9.43μmol/L,the recovery was 106.3%,and the relative standard deviation was 2.3%.
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