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山东大学学报(工学版) ›› 2017, Vol. 47 ›› Issue (4): 117-123.doi: 10.6040/j.issn.1672-3961.0.2017.002

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Fe3O4磁性石墨烯分散固相萃取水中的有机氯污染物

王明雨1,苏丽清2*,张少君1,汪昱3   

  1. 1. 山东交通学院船舶与轮机工程学院, 山东 威海 264310;2. 威海市立医院内分泌科, 山东 威海 264200;3. 山东省地方病防治研究所碘缺乏病科, 山东 济南 250014
  • 收稿日期:2017-01-03 出版日期:2017-08-20 发布日期:2017-01-03
  • 通讯作者: 苏丽清(1968— ),女,山东威海人,硕士,主要研究方向为内分泌干扰物. E-mail: ytu102@163.com E-mail:vicsee@163.com
  • 作者简介:王明雨(1974— ),男,辽宁朝阳人,教授,硕导,博士,主要研究方向为水污染控制.E-mail: vicsee@163.com
  • 基金资助:
    国家自然科学基金资助项目(51609131);山东省自然科学基金资助项目(ZR2014JL038);山东省高等学校科技计划资助项目(J14LD04;J16LA61);威海市科技发展计划资助项目(2016GGX003-1)

Fe3O4 magnetic dispersive solid-phase extraction with graphene for determination of organochlorine pesticides contaminants in water

WANG Mingyu1, SU Liqing2*, ZHANG Shaojun1, WANG Yu3   

  1. 1. Naval Architecture &
    Marine Engineering College, Shandong Jiaotong University, Weihai 264310, Shandong, China;
    2. Department of Endocrinology, Weihai Municipal Hospital, Weihai 264200, Shandong, China;
    3. Iodine Deficiency Disorders, Institute of Endemic Disease Control, Shandong Province, Jinan 250014, Shandong, China
  • Received:2017-01-03 Online:2017-08-20 Published:2017-01-03

摘要: 开发负载胶束的磁性Fe3O4纳米微粒修饰的石墨烯作为新型分散固相萃取材料,并用于水中有机氯的检测。磁性石墨烯由氧化石墨烯和Fe2+通过氧化还原法一步合成,负载阳离子表面活性剂CTAB形成纳米混合胶束作为提取系统。应用本方法分析水中的29种有机氯,检测限达到1.5~5.0 ng/L,样品加标回收率范围在75.22%~97.15%。复重性的相对标准偏差小于9.995%,与传统的固相萃取法相比,方法的灵敏度提高了50~113倍。该方法快速、灵敏、准确,可以同时测定水中多种有机氯农残,适合于大批量样品的测定。

关键词: 农药残留, 胶束提取, 分散固相萃取, 有机氯, 石墨烯, 磁性Fe3O4纳米微粒

Abstract: A novel dispersive solid-phase extraction(DSPE)analysis method was established by combining Fe3O4magnetic nanoparticles modified graphene as absorption material for determination of organochlorine pesticides(OCPs)in water. Magnetic nanoparticles modified graphene(MNG)was prepared by graphene oxide and Fe2+ through redox reaction in one step. Cationic surfactant CTAB was added as micelle forming agent, in which MNG was carrier of mixed micelles extraction system. Mixed micelle modified MNG had higher loading capacity than pure Fe3O4magnetic graphene. This method was applied to detect 29 kinds of OCPs in water. The detection limit was in the range of 1.5~5.0 ng/L. The recovery was ranged from 75.22% to 97.15%. The relative standard deviation(RSD)of repeatability was lower than 9.995%. As compared with ordinary solid-phase extraction, the sensitivity of new method increased 50~113 times. The method was suitable for simultneous determination of OCPs pesticide residues in water with high accuracy, sensitivity and less pre-treatment time, which was suitable for batch analysis of samples.

Key words: micelles extraction, Fe3O4 magnetic nanoparticles, pesticide residues, dispersive solid-phase extraction, organochlorine pesticide, graphene

中图分类号: 

  • X832
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[1] 祁振, 于淑艳, 刘璐, 王曙光*. 石墨烯对四环素的吸附热力学及动力学研究[J]. 山东大学学报(工学版), 2013, 43(3): 63-69.
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