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作 者:陶菡 黄锐 刘丰 田运霞 吴远根 TAO Han;HUANG Rui;LIU Feng;TIAN Yunxia;WU Yuangen(Key Laboratory of Fermentation Engineering and Biopharmacy of Guizhou Province,College of Liquor and Food Engineering,Guizhou University,Guiyang 550025,China)
机构地区:[1]贵州大学酿酒与食品工程学院贵州省发酵工程与生物制药重点实验室,贵阳550025
出 处:《理化检验(化学分册)》2021年第6期481-486,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:贵州省科技计划项目(黔科合LH字[2017]7294号);国家自然科学基金(31760486);贵州省科技计划项目(黔科合支撑[2019]2382号);贵州大学2017年度学术新苗培养及创新探索专项(黔科合平台人才[2017]5788)。
摘 要:以部分电化学还原的氧化石墨烯(pErGO)修饰的玻碳电极(GCE)作为工作电极(pErGO/GCE),用于苦参碱(MT)含量的电化学测定。在活化好的GCE上滴涂氧化石墨烯(GO),用恒电位法在-0.75 V下还原GCE表面的GO 200 s,得到的电极即为pErGO/GCE。以0.1 mol·L^(-1) NaH2PO4-Na2HPO4缓冲溶液(pH 7.0)作为电解质,铂丝作为对电极,Ag/AgCl作为参比电极,在开路电位下富集样品中的MT 120 s,采用差分脉冲伏安法(DPV)测定MT含量。结果显示:MT的浓度在8.0×10^(-6)~1.0×10^(-4)mol·L^(-1)内与其对应的氧化峰峰电流呈线性关系,检出限(3S/N)为4.0μmol·L^(-1)。用修饰电极重复测定MT标准溶液5次,所得测定值的相对标准偏差(n=5)为1.8%。对实际样品进行加标回收试验,回收率为94.8%~104%。方法用于实际样品分析,MT的测定值与标示值的相对偏差为-5.9%。A glassy carbon electrode(GCE)modified with partially electrochemical reduced graphene oxide(pErGO)was used as the working electrode(pErGO/GCE)for the electrochemical determination of matrine(MT).Graphene oxide(GO)was dropped on the activated GCE,and then the pErGO/GCE was obtained by reducing GO to pErGO at-0.75 V for 200 s.Using 0.1 mol·L^(-1) NaH2PO4-Na2HPO4 buffer solution(pH 7.0)as the electrolyte,platinum wire as the counter electrode and Ag/AgCl electrode as the reference electrode,MT in the sample was enriched at open circuit potential for 120 s and then determined by differential pulse voltammetry(DPV).The results showed that the concentration of MT was linearly related to its oxidation peak current in the range of 8.0×10^(-6)-1.0×10^(-4)mol·L^(-1),with detection limit(3 S/N)of 4.0μmol·L^(-1).RSDs(n=5)of the determined values was 1.8%by repeated determination of MT standard solution for 5 times with the modified electrode.Test for recovery was made on the actual samples by standard addition method,giving values of recovery in the range of 94.8%-104%.This method was used for the analysis of the actual sample,and the relative deviation between the determined value and the labeled value of MT was-5.9%.
关 键 词:部分电化学还原氧化石墨烯 电化学法 苦参碱
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