以ZIF-8为固相微萃取涂层分析环境水样中痕量多溴联苯醚  

Analysis of Polybrominated Diphenyl Ethers in Environmental Water Samples Using Zeolitic Imidazolate Framework-8 as Solid Phase Microextraction Coating

作　　者：李振[1,2] 周家斌 王霞[2] 赵汝松[2] LI Zhen;ZHOU Jia-bin;WANG Xia;ZHAO Ru-song(School of Resources and Environmental Engineering,Wuhan University of Technology,Wuhan 430070,China;Analysis and Test Center,Shandong Academy of Sciences,QILU University of Technology,Jinan 250014,China)

机构地区：[1]武汉理工大学资源与环境工程学院,湖北武汉430070 [2]齐鲁工业大学(山东省科学院分析测试中心),山东济南250014

出　　处：《分析测试学报》2018年第8期871-878,共8页Journal of Instrumental Analysis

基　　金：国家自然科学基金(21477068);山东省重点研发项目(2015GSF117011);山东省自然科学基金(ZR2015YL003;ZR2016YL003)

摘　　要：将沸石咪唑酯骨架材料(ZIF-8)制成固相微萃取涂层,结合气相色谱-三重四极杆串联质谱联用仪(GC-MS/MS),建立了一种快速灵敏分析环境水样中6种痕量多溴联苯醚的方法。采用单因素优化实验得到的最优条件为:不添加Na Cl,萃取温度为50℃,萃取时间为50 min,p H值为7.0,解吸时间和解吸温度分别为5 min和280℃。在最优条件下,该方法测定水样中多溴联苯醚的线性范围为1~1 000 ng/L,检出限为0.08~2.29 ng/L,定量下限为0.23~7.32 ng/L。日内和日间相对标准偏差分别为4.3%~6.5%和6.9%~9.3%。将该方法应用于4种实际环境水样(自来水、泉水、池塘水和垃圾填埋场废水)中多溴联苯醚的检测,回收率为81.6%~109%。A rapid and sensitive method was developed for the analysis of 6 polybrominated biphenyl ethers(PBDEs)at trace levels in environmental water samples by gas chromatography-tandem mass spectrometry(GC-MS/MS)with a synthesized zeolite imidazolate framework-8(ZIF-8)as solid phase microextraction coating.The experimental conditions were optimized with single factor tests,and the optimal conditions were as follows:extraction time:50 min,extraction temperature:50℃,pH value:7.0,desorption temperature:280℃,desorption time:5 min,and without salt addition.Under the optimized conditions,the calibration curves for 6 PBDEs were linear in the range of 1-1 000 ng/L with limits of detection and limits of quantitation of 0.08-2.29 ng/L and 0.23-7.32 ng/L,respectively.The intra-day and inter-day RSDs were in the range of 4.3%-6.5%and 6.9%-9.3%,respectively.This method was successfully applied in the analysis of PBDEs in 4 environmental water samples(tap water,spring water,pond water and landfill waste water)with recoveries of 81.6%-109%.

关 键 词：沸石咪唑酯骨架材料-8 多溴联苯醚 固相微萃取(SPME) 气相色谱-串联质谱(GC-MS/MS) 

分 类 号：O657.63[理学—分析化学] O625.22[理学—化学]