磁性功能介孔材料固相萃取-气相色谱法测定水中的多氯联苯  

Determination of polychlorinated biphenyls in water by magnetic functional mesoporous materials solid phase extraction-gas chromatography

作　　者：张利 李莉[2] 张登耀 张盛贵[1] 陈自弟 ZHANG Li;LI Li;ZHANG Dengyao;ZHANG Shenggui;CHEN Zidi(College of Food Science and Engineering,Gansu Agricultural University,Lanzhou 730070,China;College of Science,Gansu Agricultural University,Lanzhou 730070,China)

机构地区：[1]甘肃农业大学食品科学与工程学院,兰州730070 [2]甘肃农业大学理学院,兰州730070

出　　处：《分析试验室》2024年第3期409-414,共6页Chinese Journal of Analysis Laboratory

基　　金：甘肃省教育科技创新项目(GSSYLXM-02);甘肃省教育厅高等教育创新基金(2022A-062);甘肃省自然科学基金(21JR7RA806)资助。

摘　　要：采用一锅法合成Fe_(3)O_(4)纳米粒子,并利用溶胶-凝胶法制备了SBA-15@Fe_(3)O_(4)磁性介孔复合材料。以介孔二氧化硅材料(SBA-15)的表面硅羟基为靶位,借助苯基三氯硅烷与硅羟基的硅烷化反应将苯基基团接枝到材料表面,得到苯基功能化磁性介孔材料Ph-SBA-15@Fe_(3)O_(4),该材料有良好的疏水性,并保留了SBA-15的有序二维六方孔道结构。将其用于磁性固相萃取(MSPE)吸附水样中的多氯联苯(PCBs),建立了气相色谱-电子捕获检测法(GC-ECD)检测PCBs。在优化条件下,7种PCBs在0.025~50μg/L范围内呈良好线性关系,线性相关系数(R^(2))均大于0.9999,方法回收率为89.8%~108%。该方法可用于实际水样中痕量PCBs的高效快速检测。Fe_(3)O_(4) nanoparticles were synthesized by one pot method,and SBA-15@Fe_(3)O_(4) magnetic mesoporous composites were synthesized by sol-gel method.Surface silicon hydroxyl groups of mesoporous silica material(SBA-15)served as target,Ph-SBA-15@Fe_(3)O_(4) functional magnetic mesoporous material were obtained by grafting phenyl groups onto SBA-15@Fe_(3)O_(4) surface via silylation reaction between phenyl trichlorosilane and silanol group.The material not only possessed good hydrophobicity,but also retained the ordered twodimensional hexagonal pore-like structure of SBA-15.The material was used in magnetic solid-phase extraction(MSPE)pretreatment to adsorb polychlorinated biphenyls(PCBs)in water samples,and a gas chromatography method for the determination of PCBs was established.Under the optimized conditions,the seven PCBs exhibited good linear relationships in the range of 0.025-50μg/L,the correlation coefficients(R^(2))were greater than 0.9999,and the recoveries were 89.8%-108%.The MSPE method could be applied to the determination of trace PCBs in real water samples.

关 键 词：磁性固相萃取(MSPE) 多氯联苯(PCBs) 气相色谱-电子捕获检测法(GC-ECD) 

分 类 号：O657.7[理学—分析化学]