摘要
建立了一种基于共价有机框架材料的磁固相萃取-高效液相色谱方法,用于环境水样中对羟基苯甲酸酯的快速灵敏分析。首先以Fe_(3)O_(4)纳米粒子为磁核,通过1,3,5-苯三甲醛(Tb)和联苯胺(Bd)在室温下的席夫碱反应合成了磁性共价有机框架材料——Fe_(3)O_(4)@TbBd,通过扫描电镜、热重分析、X射线衍射和振动样品磁强计等表征手段证明了该磁性共价有机框架材料具有良好的热稳定性和化学稳定性,且磁响应强度较大,是用于磁固相萃取的理想材料。随后系统研究了影响萃取效率的因素,包括吸附剂用量、萃取时间、pH、解吸溶剂、解吸时间和解吸次数,建立了基于Fe_(3)O_(4)@TbBd的磁固相萃取-高效液相色谱测定环境水样中4种对羟基苯甲酸酯的方法。方法的线性范围良好,4种目标物的检出限和定量限范围分别为0.2~0.4μg/L和0.7~1.4μg/L,加标回收率为86.1%~110.8%,日内和日间精密度的相对标准偏差(RSD)分别低于5.5%和4.9%。最后将该方法应用于东湖水、长江水和生活废水中对羟基苯甲酸酯的测定,不同加标水平下对羟基苯甲酸酯的回收率在80.7%~117.5%之间,RSD在0.2%~8.8%之间。该方法操作简单,萃取时间短,灵敏度较高且对环境友好,在环境水样中对羟基苯甲酸酯的检测方面有良好的应用潜力。
Parabens are a class of antimicrobial preservatives that are widely used in cosmetics, pharmaceuticals, and food products because of their ease of production, antimicrobial effect, and low price. The widespread use of these parabens, poses potential risks to human health. Therefore, it is necessary to establish a simple and rapid method for the detection of parabens. The large number of substrate interferences in complex samples is an important factor affecting the sensitivity of analytical methods. Magnetic solid-phase extraction(MSPE) has received much attention because of its advantages of easy operation, short extraction time, small sample amount, low cost, and environmental friendliness. Covalent organic frameworks(COFs) with high crystallinity, high specific surface area, adjustable pore size, regular porosity, as well as high chemical and thermal stability are now widely used in separation and analysis. Therefore, a sample pretreatment method combining MSPE and COF for the analysis of parabens in complex matrices is very promising. A magnetic covalent organic framework, Fe_(3)O_(4)@TbBd, was successfully synthesized by the Schiff base reaction of 1,3,5-triformylbenzene(Tb) and benzidine(Bd) at room temperature using FeOnanoparticles as magnetic cores. Characterization by scanning electron microscopy(SEM), thermogravimetric analysis(TGA), X-ray diffraction(XRD), vibrating sample magnetometer(VSM) measurements, etc. revealed that the magnetic COF has high magnetic responsiveness, as well as good thermal and chemical stability, which make it an ideal adsorbent for the MSPE of parabens. Some factors related to the extraction efficiency, including the amount of adsorbent, extraction time, pH, desorption solvent, desorption time, and number of desorption were systematically investigated. A method involving MSPE and high performance liquid chromatography-ultraviolet detection(HPLC-UV) based on the Fe_(3)O_(4)@TbBd was developed for the determination of four parabens(ethylparaben, propylparaben, butylparaben, and
作者
包月
翟怡鑫
宁涛
陈品
朱书奎
BAO Yue;ZHAI Yixin;NING Tao;CHEN Pin;ZHU Shukui(State Key Laboratory of Biogeology and Environmental Geology,China University of Geosciences,Wuhan 430074,China)
出处
《色谱》
CAS
CSCD
北大核心
2022年第11期1005-1013,共9页
Chinese Journal of Chromatography
基金
湖北省生态环境厅环保科研项目(2017HB04)
中央高校基本科研业务费项目(CUG170102)。
关键词
共价有机框架
磁固相萃取
高效液相色谱
对羟基苯甲酸酯
环境水样
covalent organic framework(COF)
magnetic solid-phase extraction(MSPE)
high performance liquid chromatographic(HPLC)
parabens
environment water
