摘要
采用水热法合成了酮胺型共价有机骨架材料(TpBD),硅酮胶黏附法制得固相微萃取纤维涂层,探究了该涂层对水中多溴联苯醚(PBDEs)的萃取性能.利用正交实验优化了TpBD涂层的萃取条件,结合气相色谱技术建立了基于该涂层的水体PBDEs定量分析方法.研究结果显示,TpBD涂层不但具有良好的热稳定性和化学稳定性,还可高效富集水中的PBDEs,在相同萃取条件下,TpBD涂层对PBDEs的萃取效率是商用涂层的1.2—39.5倍.基于TpBD涂层的PBDEs检测方法线性范围较宽(2.00—50.00 ng·L^(−1))、灵敏度高(检出限为0.16—0.45 ng·L^(−1))、精密度和重现性好(同批次涂层测定结果的日内相对标准偏差(RSD)<14.7%,日间RSD<13.5%;3批次涂层测定结果的RSD<13.1%),在实际环境水样的分析中表现出良好的适用性(加标回收率为81.1%—106.5%).
In this study,aβ-ketoenamine-linked covalent organic framework(TpBD)coating was applied for the solid-phase microextraction(SPME)of polybrominated diphenyl ethers(PBDEs)in water.The TpBD was prepared by the hydrothermal method and was coated on a stainless steel wire by physical adhesion using silicone glue.The PBDE analysis method was established by coupling the TpBD coated fiber with gas chromatography.The extraction conditions were optimized using the orthogonal experiment.The TpBD coating not only had good thermal and chemical stabilities,but also afforded high extraction efficiency for PBDEs(1.2—39.5 times higher than commercial coatings).The method based on TpBD coated fiber for PBDE determination exhibited relatively wide linear ranges(2.00—50.00 ng·L^(−1)),high sensitivity(detection limits of 0.16—0.45 ng·L^(−1)),high precision(intra-day relative standard deviations(RSD)<14.7%and inter-day RSD<13.5%),good reproducibility(RSD<13.1%),and good recoveries(81.1%—106.5%)in real water samples.
作者
李玉凡
马璞
陶庆文
付翯云
LI Yufan;MA Pu;TAO Qingwen;FU Heyun(School of Environment,State Key Laboratory of Pollution and Resource Reuse,Nanjing University,Nanjing,210093,China)
出处
《环境化学》
CAS
CSCD
北大核心
2023年第7期2340-2348,共9页
Environmental Chemistry
基金
国家重点研究计划(2019YFC1804201)
江苏省自然科学基金(BK20190059)资助.
关键词
多溴联苯醚
共价有机骨架
固相微萃取
气相色谱.
polybrominated diphenyl ethers
covalent organic framework
solid-phase microextraction
gas chromatography.
