石墨烯固相微萃取纤维的制备及对多氯联苯的检测  

Preparation of Graphene-based Solid Phase Microextraction Fiber and Its Determination of Polychlorinated Biphenyls

作　　者：贾其娜[1] 赵广超[1] 

机构地区：[1]安徽师范大学环境科学与工程学院,安徽芜湖241000

出　　处：《分析测试学报》2013年第5期541-546,共6页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(20975001)

摘　　要：采用溶胶-凝胶方法合成了石墨烯复合材料,将其均匀地涂在铜丝表面制备了石墨烯固相微萃取纤维,结合固相微萃取-气相色谱-电子捕获检测器(SPME-GC-ECD)技术,建立了对环境中类二英多氯联苯(DL-PCBs)的直接测定方法。实验优化了萃取温度、萃取时间、pH值和离子强度等固相微萃取条件。在优化条件下,石墨烯固相微萃取纤维较商品化纤维(100μm PDMS、75μm CAR/PDMS、85μm PA)的萃取效率平均高2倍。对于DL-PCBs分析,该方法在0.05～3.5μg.L-1范围内呈良好线性(除PCB169外,r2均高于0.99),检出限为4.7～8.8 ng.L-1,单个纤维间及纤维与纤维间的相对标准偏差分别为1.4%～8.1%和2.4%～12.8%。该纤维对12种环境样品中DL-PCBs加标0.5μg.L-1和2 ng.g-1的回收率为87%～120%。方法简单、快速、灵敏,可实现对多氯联苯的痕量检测。A novel graphene-based solid phase microextraction（SPME） fiber was prepared by coating graphene composite onto the surface of a treated copper wire using sol-gel method,and was applied in the direct determination of dioxin-like polychlorinated biphenyls（DL-PCBs） in the environmental samples,combining solid phase microextraction-gas chromatography-electron capture detector（SPME-GC-ECD） technology.The parameters influencing the extraction and efficiency,including extraction temperature,extraction time,sample pH,salt concentration and desorption time,were optimized.Under the optimized conditions,the chromatographic peak areas obtained from the graphene-based fiber extracting twelve DL-PCBs were averagely two times higher than those obtained from the commercial fibers such as 100 μm PDMS,75 μm CAR/PDMS,85 μm PA.The graphene-based fiber showed good linearity for DL-PCBs in the range of 0.05-3.5 μg·L-1 with correlation coefficients higher than 0.99 except PCB169（r2=0.987 4）.The limits of detection（LODs） were in the range of 4.7-8.8 ng·L-1.The relative standard deviations（RSDs） were 1.4%-8.1% for a single fiber and 2.4%-12.8% for fiber-to-fiber.The average recoveries of twelve DL-PCBs were in the range of 87%-120% with spiked levels of 0.5 μg·L-1 for DL-PCBs standard in the environmental water samples and 2 ng·g-1 in the environmental mud samples.The proposed method was simple,sensitive and rapid,and could be used for the detection of trace amount of DL-PCBs.

关 键 词：固相微萃取 石墨烯 多氯联苯 环境样品 

分 类 号：O657.71[理学—分析化学] TQ241.31[理学—化学]