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作 者:刘梦琴 向亨芳 曾荣英 LIU Meng-qin;XIANG Heng-fang;ZENG Rong-ying(Key Laboratory of Functional Organometallic Materials of College of Hunan Province,College of Chemistry and Materials Science,Hengyang Normal University,Hengyang Hunan 421008,China)
机构地区:[1]衡阳师范学院化学与材料科学学院,功能金属有机材料湖南省重点实验室,湖南衡阳421008
出 处:《衡阳师范学院学报》2020年第3期76-81,共6页Journal of Hengyang Normal University
基 金:湖南省教育厅项目(19K011、18A336、GN19K04);衡阳市科技计划项目(2019jhzx0741)。
摘 要:文章通过hummers法制备了氧化石墨烯(GO),将氧化石墨烯和羧基化多壁碳纳米管(MWCNTs)在水合肼中还原得到石墨烯/碳纳米管复合材料,采用滴涂法制备石墨烯/碳纳米管复合修饰电极(GR/MWCNTs/GCE)。用循环伏安法(CV)和差分脉冲溶出伏安法(DPSV)研究了大黄素在该修饰电极上的电化学行为。结果表明:在pH=5.00的混合磷酸盐(PB)缓冲液中,0^-0.8 V电位范围,以100 mV/s速率扫描,在-0.65 V附近出现明显的还原峰,其峰电流与大黄素的浓度在1×10^-8~1×10^-5mol/L内具有良好的线性关系,检出限(S/N=3)为1.1×10^-9mol/L。该修饰电极制备简便,测定大黄素灵敏、快速、选择性好。测定大黄药材中的大黄素回收率为96.0~103.0%,相对标准偏差(RSD)为1.7~3.5%,为大黄素的痕量分析提供了一种新方法。In this paper,graphite oxide(GO)was prepared by Hummers method,and graphite oxide and carboxyl multi-walled carbon nanotubes(MWCNTs)were reduced in hydrazine hydrate to obtain graphene/carbon nanotubes composites,and the graphene/carboxyl multi-walled carbon nanotubes composite modified electrode(GR/MWCNTs/GCE)was prepared by drop casting.The electrochemical behavior of emodin at the electrode was studied by cyclic voltammetry(CV)and differential pulse stripping voltammetry(DPSV).The results showed that in the phosphate buffer at pH=5.00,when the potential was scanned in the range of 0^-0.8 V at a rate of 0.1 V/s,there was a clear reduction peak around-0.65 V and a good linear relationship between the peak current and emodin concentration at 1×10^-8 to 1×10^-5 mol·L^-1 was obained,the linear equation is Ip(μA)=1.1285c(μmol/L)+4.7699,r=0.9929,and the detection limit(S/N=3)is 1.1×10^-9 mol/L.The modified electrode was easy to prepare,and the determination of emodin was sensitive rapid and selective.The recovery rate of emodin in rhubarb was 96.0~103.0%,and the relative standard deviation(RSD)was 1.7~3.5%.Therefore,a new method for trace analysis of emodin based on the GR/MWCNTs/GCE is provided.
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