摘要
目的构建一种新型电化学传感器,并用于快速检测食品包装中的对特辛基苯酚[p-(tert-octyl)phenol,POP]。方法利用溶剂热法合成铋镍双核金属有机骨架(bismuth nickel bimetallic metal-organic frameworks,Bi-Ni-BTC),通过超声自组装的方法将Bi-Ni-BTC与多壁碳纳米管(multi walled carbon nanotubes,MWCNTs)制备复合材料Bi-Ni-BTC@MWCNTs,并滴涂成膜于玻碳电极(glassy carbon electrode,GCE)表面,构建电化学传感器Bi-Ni-BTC@MWCNTs/GCE。采用循环伏安法、电化学阻抗谱法、扫描电子显微镜、X-射线衍射、傅立叶红外光谱等方法进行表征分析,并通过可行性实验初步评价该传感器的性能。使用线性扫描伏安法(linear sweep voltammetry,LSV),通过调整配体比例、修饰量、缓冲溶液的种类、pH、富集时间、富集电位、扫描速度等优化传感器的性能。结果GCE表面上滴涂电极修饰液3次,共3层,修饰量共18μg、pH 7.0磷酸盐缓冲盐溶液、扫描速率100 mV/s、富集电位0.3 V、富集时间120 s条件下,POP的峰电流(ΔI)与浓度(C)间的线性回归方程:ΔI=0.87931C+5.29413(r2=0.9964),POP的检测浓度范围为1.0~100.0μmol/L,检出限为68 nmol/L(3σ/K)。该电化学传感器应用于食品包装袋迁移出的POP时,其加标回收率为95.39%~100.81%,相对标准偏差为0.81%~5.93%(n=5)。结论本研究制备的铋镍双金属有机骨架复合材料制备过程简单、成本低,可用于POP的超灵敏检测。
Objective To construct a new type of electrochemical sensor for the rapid detection of p-(tert-octyl)phenol(POP)in food packaging.Method Bismuth nickel bimetallic metal-organic frameworks(Bi-Ni-BTC)were synthesized by solvothermal method,and the composite material Bi-Ni-BTC@MWCNTs was prepared by ultrasonic self-assembly of Bi-Ni-BTC and multi-walled carbon nanotubes(MWCNTs).The electrochemical sensor Bi-Ni-BTC@MWCNTs/GCE was constructed by drop-coating the film on the surface of a glassy carbon electrode(GCE).Characterization and analysis were performed by cyclic voltammetry,electrochemical impedance spectroscopy,scanning electron microscopy,X-ray diffraction,Fourier transform infrared spectroscopy.The performance of the sensor was preliminarily evaluated by feasibility experiments.The performance of the sensor was optimized by adjusting the ligand ratio,modification amount,buffer solution type,pH,accumulation time,accumulation potential,scan rate by linear sweep voltammetry(LSV).Results Three layers of electrode modification solution were drop-coated on the GCE surface,with a total modification amount of 18μg,pH 7.0 phosphate buffered saline solution,scan rate 100 mV/s,enrichment potential 0.3 V,enrichment time 120 s.Under these experimental conditions,the linear regression equation between the peak current(ΔI)and concentration of POP wasΔI=0.87931C+5.29413(r2=0.9964),with a detection concentration range of 1.0‒100.0μmol/L and a limit of detection of 68 nmol/L(3σ/K).When applied to POP migrated from food packaging bags,the recoveries were 95.39%‒100.81%,with a relative standard deviation of 0.81%‒5.93%(n=5).Conclusion This study has proposed a new strategy for ultra-sensitive detection of POP using a bismuth nickel bimetallic metal-organic framework composite material with simple preparation process and low cost.
作者
林谦
郑仲龙
黄迪惠
LIN Qian;ZHENG Zhong-Long;HUANG Di-Hui(Food Flexible Packaging Technology Fujian University Engineering Research Center,Fujian Polytechnic Normal University,Fujian Province-Indonesia Marine Food Joint Research and Development Center,Fujian Polytechnic Normal University,Fuqing 350300,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2023年第19期98-106,共9页
Journal of Food Safety and Quality
基金
福建省科技厅自然科学基金项目(2020J01310、2022J01977)。
关键词
对特辛基苯酚
铋镍双金属有机骨架
多壁碳纳米管
电化学传感器
线性扫描伏安法
食品包装袋
p-(tert-octyl)phenol
bismuth nickel bimetallic metal-organic frameworks
multi walled carbon nanotubes
electrochemical sensor
linear sweep voltammetry
food packaging bag