石墨烯基固相微萃取涂层的制备及其对多溴联苯的检测

Preparation Graphene-Based Solid Phase Microextraction Fiber and Determination of Polybrominated Biphenyls

采用直接涂层的方法将石墨烯纳米材料均匀地涂布在铜丝表面制得了石墨烯基固相微萃取涂层纤维,结合固相微萃取-气相色谱-电子捕获检测器(SPME-GC-ECD)技术,建立了对水中多溴联苯(PBBs)的直接测定方法。实验优化了萃取时间、萃取温度、离子强度等固相微萃取条件。在优化的条件下,该方法在20-2000ng·L-1的范围内表现出了良好的线性,检出限为5.2-10.2ng·L-1;单个纤维间和纤维与纤维间的精密度分别为4.84-9.96%和8.3-12.4%。纤维对环境样品中PBBs加标2μg·L-1的回收率为94.5-111%。该方法简单、快速、灵敏,可实现多溴联苯的快速检测。

A novel graphene-based solid phase microextraction -iSPME） fiber was prepared by coating graphene onto the surface of a treated cooper wire using direct coating method, then it was applied to determination polybrominated biphenyls （PBBs） of the environmental samples combining solid phase microextraction-gas chromatography-electron capture detector （SPME-GC-ECD） technology. The parameters which influence the extraction efficiency, including extraction time, extraction temperature, salt concentration were optimized. Under the optimized condition, the graphene-based fiber showed a good linearity ranged from 20 to 2000ng·L-1. The limits of detection （LODs） were in the range of 5.2-10.2ng·L -1. The relative standard deviations （RSD%） were found to be in the range of 4.84-9.96% for a single fiber and 8.3-12.4% for fiber-to-fiber. The relative recoveries of twelve PBBs were 94.5-111% with spiked 2μg·L-1 of PBBs standard in the environmental water samples. In this work, the proposed method was simple, sensitive, rapid for PBBs analysis.