不同活化方法修饰碳电极检测红油中辣椒素含量的电化学研究  

Electrochemical Study on the Detection of Capsaicin in Red Oil by Modified Carbon Electrode with Different Activation Methods

作　　者：陆超群 陈星光 恽宁 顾千辉 LU Chaoqun;CHEN Xingguang;YUN Ning;GU Qianhui(Three Squirrels Co.,Ltd.,Wuhu 241000,China;School of Food Science,Jiangnan University,Wuxi 214000,China;School of Food Science,Nanchang University,Nanchang 330000,China)

机构地区：[1]三只松鼠股份有限公司,安徽芜湖241000 [2]江南大学食品学院,江苏无锡214000 [3]南昌大学食品学院,江西南昌330000

出　　处：《食品工业科技》2023年第17期297-305,共9页Science and Technology of Food Industry

基　　金：2021年“十四五”国家重点研发计划(2021YFD210020501)。

摘　　要：研究酸、碱、盐活化方法对不同碳电极检测辣椒素类物质含量的影响,制备活化碳电极传感器,用于检测红油中辣椒素类物质的含量,并探究其检测机理。以盐酸、氢氧化钠、磷酸盐溶液为活化液,分别对玻碳电极和石墨电极进行活化,以活化电极作为电化学传感器检测红油中辣椒素含量,对比不同活化条件对检测效果的影响。通过电化学实验、扫描电镜和拉曼光谱探究辣椒素的电化学检测机理。结果表明,活化能够显著增强电极对辣椒素的检测灵敏度。其中,磷酸盐活化法为最佳活化方法,活化后的石墨电极对辣椒素类物质的检测性能最佳。制备磷酸盐活化石墨电极的最优条件为:磷酸盐浓度0.2 mol/L、pH5.0、电位范围-2.0~2.2 V、扫描段数20。在此条件下,辣椒素的响应电流比活化前提高了11.2倍,反应过程为受扩散控制的氧化还原反应。此外,活化后的石墨电极表面氧元素含量从0.8%增加至34.9%。其检测机理为辣椒素得失电子产生电信号,并通过磷酸盐活化增加电极表面含氧基团提高检测灵敏度。基于磷酸盐活化石墨电极的传感器得到的红油中辣椒素含量的线性范围为5~80μmol/L,检测限为2.30μmol/L,加标回收率为98.23%~112.60%,结果与液质联用检测红油中辣椒素含量相比误差小于10%,并具有良好的抗干扰能力与稳定性。利用磷酸盐活化石墨电极构建传感器对红油中辣椒素含量进行检测具有简单、经济、有效的特点,该方法可以为生产实践提供一定参考。To study the effects of acid,alkali and salt activation methods on the detection of capsaicin by different carbon electrodes,and prepare activated carbon electrode sensors to detect the content of capsaicin in red oil and explore the mechanism.In this work,the glassy carbon electrode and graphite electrode were activated by hydrochloric acid,sodium hydroxide,and phosphate solution respectively.Then,the activated electrodes were used as electrochemical sensors to detect the content of capsaicin in red oil,and the effect of activation conditions on detection performance was studied.Subsequently,the electrochemical detection mechanism of capsaicin was investigated by electrochemical experiments,scanning electron microscopy and Raman spectroscopy.According to the results,activation can significantly enhance the detection sensitivity of the electrode to capsaicin.Among them,phosphate activation method was the best activation method,and the activated graphite electrode showed the best detection performance for capsaicin.The optimum preparation conditions of phosphate activated graphite electrode were as follows:the phosphate concentration was 0.2 mol/L,the pH was 5.0,the potential range was−2.0~2.2 V,and the number of scanning segments was 20.Under this condition,the response current of capsaicin was 11.2 times higher than that before activation,and the reaction process was a redox reaction controlled by diffusion.Additionally,the surface oxygen content of activated graphite electrode increased from 0.8%to 34.9%.The detection mechanism was that capsaicin gains and loses electrons to generate electrical signals,and increases the oxygen containing groups on the electrode surface through phosphate activation to improve the detection sensitivity.The linear range of capsaicin content in red oil obtained by phosphate activated graphite electrode was 5~80μmol/L,detection limit was 2.30μmol/L,the recovery rate of spiking was 98.23%~112.60%,the error was less than 10%compared with LC-MS,and the sensor had good anti-interfer

关 键 词：活化方法 电化学传感器 石墨电极 辣椒素 检测机理 红油 

分 类 号：TS207.3[轻工技术与工程—食品科学]