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作 者:白小慧[1] 杜芳艳[1] 陈娟[1] 李霄[1] 高立国[1] 李真真 Bai Xiaohui;Du Fangyan;Chen Juan;Li Xiao;Gao liguo;Li Zhenzhen(College of Chemistry and Chemical Engineering,Yulin University,Yulin,Shaanxi 719000,China)
机构地区:[1]榆林学院化学与化工学院
出 处:《化学世界》2019年第12期870-876,共7页Chemical World
基 金:榆林市科技计划(No.2016CXY-09);榆林学院2014年(No.14yk24)资助项目
摘 要:采用电沉积法结合表面滴涂法制备了纳米氧化镍/单壁碳纳米管修饰玻碳电极(NiOx/SWCNTs/GCE),通过循环伏安法、扫描电子显微镜对修饰电极进行了表征,运用方波伏安法和循环伏安法研究了木犀草素在NiOx/SMWCNTs/GCE修饰电极上的电化学行为。结果表明,电极表面纳米氧化镍和单壁碳纳米管的存在对木犀草素具有良好的电催化活性,电极稳定性高,表面可以更新。在pH 2.8±0.2的伯瑞坦-罗宾森缓冲溶液中,木犀草素在NiOx/SWCNTs/GCE修饰电极上的氧化、还原峰电位均负移,峰电流明显增加,据此,建立了测定木犀草素的方法。在-0.2~0.6 V电位区间内,在方波伏安曲线上的还原峰电位E为0.43 V,峰电流I木犀草素浓度在2.4×10^-6~1.0×1.0^-10 mol/L范围内与电位有良好的线性关系,线性回归方程为I=5.39×10^6c+4.1716,R^2=0.999,检出限(3S/N)为3.4×10^-11 mol/L,此方法用于砂珍棘豆中木犀草素含量的测定。样品回收率为98.69%~104.40%,相对标准偏差为1.05%~1.37%。NiOx/SWCNTs/GCE was synthesized by electro-deposition and drop-coating method,which was characterized by cyclic voltammetry(CV)and scanning electron microscope(SEM).What’s more,the electrochemical behavior of luteolin was studied by square wave voltammetry and voltammetry on the NiOx/SWCNTs/GCE,respectively.The result showed when the nano NiO and single-walled carbon nanotubes was both existed on the electrode surface,the luteolin exhibited excellent electro-catalytic activity,high electrode stability and its surface was renewable.The oxidation and reduction peak potentials of luteolin on NiOx/SWCNTs/GCE modified electrodes were appeared negatively shifted and the peak current increased significantly when in Britton-Robinson buffer solution with pH 2.8±0.2 respectively,thus a new method for the determination of luteolin was established.The reduction peak potential(E)of luteolin in square wave voltammetry curve was 0.43 V in the range of-0.2~0.6 V potential.The peak current concentration(I)had a good linear relationship with the potential in the range of 2.4×10^-6~1.0×1.0^-10 mol/L.Meanwhile,the linear regression equation was I=5.39×106c+4.1716,R^2=0.999 and the detection limit(3S/N)was 3.4×10^-11 mol/L.Therefore,this method can be used for the determination of luteolin content in Oxytropis racemosa.The recovery ratio of sample was ranged from 98.69%to 104.40%while the relative standard deviation was ranged from 1.05%to 1.37%.
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