| 石墨烯固相微萃取纤维的制备及对多氯联苯的检测 |
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| 基金项目:国家自然科学基金资助项目(20975001) |
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| 中文摘要: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(100 μm PDMS、75 μm CAR/PDMS、85 μm PA)的萃取效率平均高2倍。对于DL-PCBs分析，该方法在0.05~3.5 μg?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0.5 μg?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。 |
| 中文关键词:固相微萃取 石墨烯 多氯联苯 环境样品 |
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| Preparation of Graphene-based Solid Phase Microextraction Fiber and ItsDetermination of Polychlorinated Biphenyls |
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| Abstract:A novel grapheme-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 grapheme-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 grapheme-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. |
| Key Words:solid phase microextraction graphene polychlorinated biphenyls environmental sample |
| 引用本文：贾其娜，赵广超.石墨烯固相微萃取纤维的制备及对多氯联苯的检测[J].分析测试学报,2013,32(5):541-546. |
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