摘要
以溶剂热法制备磁性MIL-100(Fe)微粒,并应用于黄瓜中氯吡脲的磁固相萃取(MSPE).通过透射电镜、热重分析和傅里叶红外光谱仪对材料进行表征.该磁微粒在水溶液中显示出优异的分散性.研究磁微粒用量、样品溶液pH、盐度和解吸溶剂体积对磁萃取的影响.在最佳的萃取条件下,建立黄瓜中氯吡脲残留的MSPE-HPLC定量分析方法,该方法的线性范围为5~500μg·kg^(-1),相关系数(R^(2))为0.9992.检测限(LOD)为1.4μg·kg^(-1),日间和日内精密度(RSD,n=4)小于8.8%.将该方法应用于实际样品分析,结果符合GB 23200.110—2018的精密度要求.
Magnetic MIL-100@Fe_(3)O_(4)(Fe)microspheres were synthesized using solvothermal method and supplied for magnetic solid-phase extraction(MSPE)of forchlorfenuron in cucumber.The materials were characterized by transmission electron microscope,thermogravimetry and Fourier transform infrared spectrometer.The magnetic microparticles showed excellent dispersibility in aqueous solution.The factors influencing the extraction,including the amount of magnetic microspheres,sample pH,salt concentration of sample solution,and the volume of desorption solvent were investigated in detail.Under the optimum conditions,an MSPE-HPLC method was developed for the determination of forchlorfenuron in cucumber.The linear range of the method was 5~500μg·kg^(-1) with the correlation coefficient(R^(2))of 0.9992.The limit of detection was 1.4μg·kg^(-1).The intra-day and inter-day precision(RSD,n=4)were less than 8.8%.The method was applied in the analysis of real sample,and the result was satisfied.
作者
吴官永
王筱倩
党雪平
陈怀侠
WU Guanyong;WANG Xiaoqian;DANG Xueping;CHEN Huaixia(College of Chemistry and Chemical Engineering,Hubei University, Wuhan 430062, China)
出处
《湖北大学学报(自然科学版)》
CAS
2022年第3期265-269,共5页
Journal of Hubei University:Natural Science
基金
国家自然科学基金(21804034)资助。