基于聚鸟氨酸修饰的玻碳电极用循环伏安法测定盐酸肾上腺素注射液中肾上腺素的含量  

Determination of Epinephrine in Epinephrine Hydrochloride Injection by Cyclic Voltammetry Based on Glassy Carbon Electrode Modified with Polyornithine

作　　者：吕惠萍 马心英 陈美凤 朱琪 曾会青 Lü Huiping;MA Xinying;CHEN Meifeng;ZHU Qi;ZENG Huiqing(College of Chemistry and Chemical Engineering,Heze University,Heze 274015,China)

机构地区：[1]菏泽学院化学化工学院,菏泽274015

出　　处：《理化检验（化学分册）》2022年第5期506-511,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：玻碳电极(GCE)经抛光、清洗干净、干燥后,放入含1.0×10^(-4)mol·L^(-1)鸟氨酸的磷酸盐缓冲溶液(PBS,pH 8.0)中,以GCE为工作电极、Ag/AgCl电极为参比电极、铂丝电极为对电极,在10 mV·s^(-1)扫描速率下于-1.8~2.3 V内循环扫描12段,取出修饰后的电极,用水清洗、干燥后即得聚鸟氨酸修饰的玻碳电极(POrn/GCE)。取盐酸肾上腺素注射液(1 mL∶1 mg) 0.72 mL,用PBS稀释至50 mL,分取10 mL置于25 mL的小烧杯中,搅拌130 s,以POrn/GCE为工作电极的三电极体系下进行循环伏安法(CV)扫描,扫描电位为-0.4~1.0 V,扫描速率为0.08 V·s^(-1)。结果显示:肾上腺素在POrn/GCE上的氧化/还原峰电位(E_(pa)、E_(pc))和在GCE上的基本一致,氧化/还原峰电流(|i_(pa)|、i_(pc))分别为39.9,15.6μA,较GCE上的(15.3,1.66μA)明显增加,同时,溶剂对肾上腺素的测定无干扰,说明修饰电极对肾上腺素具有较好的电催化作用;E_(pa)与pH呈负相关线性关系,曲线斜率的绝对值(0.058 7)接近0.059,说明电极反应是一个有质子参与的过程,且参与反应的质子数和电子数相同;|i_(pa)|与扫描速率呈线性关系,说明电极反应过程由吸附控制。肾上腺素的浓度在2.0~100μmol·L^(-1)内与其对应的|i_(pa)|呈线性关系,检出限为0.13μmol·L^(-1);100倍的尿素、色氨酸、甘氨酸和赖氨酸,50倍的Cd^(2+)和Ca^(2+),10倍的Al^(3+)和Fe^(3+)都不干扰肾上腺素的测定;用修饰电极重复分析标准溶液6次,测定值的相对标准偏差(RSD)为3.9%,将修饰电极放置7 d,|i_(pa)|较初始值减少了不到3.0%;对实际样品进行加标回收试验,测定值与标签值基本一致,回收率为97.6%~102%。After GCE was polished,cleaned and dried,it was put into phosphate buffer solution(PBS,pH 8.0)containing 1.0×10^(-4)mol·L^(-1) ornithine,with GCE as working electrode,Ag/AgCl electrode as reference and platinum wire electrode as the counter electrode.At the scanning rate of 10 mV·s^(-1),the GCE was modified by cyclic voltammetry(CV)in the range of^(-1).8-2.3 V for 12 segments.The modified electrode was taken out,washed with water and dried,and POrn/GCE was obtained.0.72 mL of epinephrine(EP)hydrochloride injection(1 mL∶1 mg)was taken,diluted to 50 mL with PBS.An aliquot(10 mL)was taken into a 25 mL-small beaker,and stirred for 130 s.CV scanning was performed in three-electrode system with POrn/GCE as the working electrode,the scanning potential was-0.4-1.0 V,and the scanning rate was 0.08 V·s^(-1).It was shown that the oxidation/reduction peak potentials(E_(pa)/E_(pc))of EP on POrn/GCE were basically the same as those on GCE,and the oxidation/reduction peak currents(|i_(pa)|,i_(pc))were 39.9,15.6μA,which were higher than those(15.3,1.66μA)on GCE,and the solvent did not interfere with the determination of EP,indicating that the modified electrode had a better electrocatalytic effect on EP;E_(pa) had a negative linear relationship with pH,and the absolute value of the slope(0.0587)of the curve was close to 0.059,indicating that the electrode reaction was a process involving protons,and the number of protons and electrons involved in the reaction was the same;the|i_(pa) |had a linear relationship with the scanning rate,indicating that the electrode reaction process was controlled by adsorption.Linear relationship between values of concentration and|i_(pa) |of EP was kept in the range of 2.0^(-1)00μmol·L^(-1),with detection limit of 0.13μmol·L^(-1);100 times of urea,tryptophan,glycine and lysine,50 times of Cd^(2+)and Ca^(2+),10 times of Al^(3+)and Fe^(3+)did not interfere with the determination of EP.Repeated analysis of the standard solution with the modified electrode was made 6 times,and RSD of the de

关 键 词：聚鸟氨酸 修饰电极 循环伏安法 肾上腺素 盐酸肾上腺素注射液 

分 类 号：O657.14[理学—分析化学]