纳米铜/石墨烯修饰电极用于离子交换色谱测定五种单糖  

Ion-exchange Chromatography with Electrochemical Detection Using Copper Nanoparticles/Graphene Composite Film Modified Electrode for Determination of Monosaccharide

作　　者：王凤丽[1] 汪凤梅[2] 习玲玲[1] 朱作艺[1] 黄忠平[1] 朱岩[1] 

机构地区：[1]浙江大学西溪校区化学系,杭州310028 [2]浙江大学医学院附属妇产科医院,杭州310006

出　　处：《分析化学》2013年第10期1601-1605,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.207750570);浙江省自然科学基金(Nos.Y407153;Y4100190)资助

摘　　要：把纳米铜和石墨烯修饰在玻碳电极表面，制备了纳米铜／石墨烯复合修饰电极。采用电化学方法，在-1．5—0V的循环扫描电位条件下，氧化石墨烯（GO）和Cu^2＋同时在玻碳电极上被电化学还原，形成石墨烯（Gr）和纳米铜（CuNPs）复合膜。所制备的修饰电极对葡萄糖等单糖化合物具有较高的电催化活性，且电极稳定性和重现性均良好。将此修饰电极作为电化学检测器，与高效阴离子交换色谱联用，分离测定了5种单糖化合物（岩藻糖、阿拉伯糖、半乳糖、葡萄糖和甘露糖）。结果表明，岩藻糖和阿拉伯糖的线性范围为0．1～100mg／L，半乳糖、葡萄糖和甘露糖的线性范围为0．5～100mg／L，5种单糖化合物的线性相关系数均大于0．998，相对标准偏差RSD（n=6）为1．9％～2．5％，检出限在0．02～0．10mg／L之间；将此方法用于测定样品桑黄粗多糖的单糖组成，测得5种单糖的回收率为84．8％-94．5％，准确度和精密度均较好。A novel copper nanoparticles/graphene modified glassy carbon electrode （CuNPs-Gr/GCE） was constructed. The CuNPs-Gr nanoeomposite was prepared by simultaneous electrochemical reduction using graphene oxide （GO） and copper ion as the starting materials under cyclic potential from -1.5 to 0 V. The modified electrode showed prominent electrocatalytic oxidation towards monosaccharide. Employing the CuNPs- Gr/GCE as an amperometric detector for high performance anion-exchange chromatography （HPIC）, five monosaccharides （fucose, arabinose, galactose, glucose and mannose ） were analyzed on-line with good reproducibility and stablity. Under constant applied potential of ＋0.55 V （vs Ag/AgC1）, the detection limits （S/N= 3 ） of the all investigated compounds were at the level of 0.02-0.10 mg/L. The dynamic linear ranges spanned generally three orders of magnitude with correlation coefficients more than 0. 998, and the RSDs （ n = 6） range from 1. 9% to 2. 5%. The analytical method has successfully been applied to determine the monosaccharide composition of crude polysaccharide from phellinus igniarius with acceptable level of sensitivity and recovery （from 84.8% to 94.5% ）. As a result, the proposed method appears to be useful and effective for the routine practical determinations of common carbohydrates in real matrices without derivatization procedures.

关 键 词：纳米铜 石墨烯 离子交换色谱 电化学 单糖化合物 

分 类 号：O657.75[理学—分析化学]