Synthesis of Fe3O4/ reduced Graphene Oxide and its application in the determination of Organophosphorus Pesticide
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摘要: 本文采用一步溶剂热法合成了基于石墨烯的磁性纳米复合物(石墨烯/四氧化三铁,G-Fe3O4),并作为一种有效的吸附剂应用于环境样品中一些有机磷农药(二嗪农,甲基对硫磷,甲基嘧啶磷,水胺硫磷和喹硫磷)的分离富集,气相色谱检测分析。该方法集石墨烯的高吸附量和Fe3O4易回收于一体,能避免传统固相萃取方法(如离心和过滤)的时间耗损。本文考察了不同的实验参数对磁性纳米复合物萃取效率的影响,主要包括复合物的量、萃取时间、离子强度以及解吸条件。最佳萃取条件为:复合物量为20mg;萃取时间为15min;Na Cl浓度为0.5%;洗脱溶剂为乙腈以及洗脱剂的量为1.5m L。在最优条件下,该方法的线性相关系数在0.99850.9996之间,五种有机磷的检测限LOD在0.00020.009ng/m L之间,连续5次重复操作所得相对标准偏差RSD为3.2%7.8%,结果表明该磁性固相萃取吸附剂在农药的富集分离中有很好的应用前景。Abstract: A graphene- based magnetic nanocomposite ( graphene- ferriferrous oxide, G- Fe3O4) was synthesized by one- pot solvothermal method and used as an effective adsorbent for the preconcentration of someorganophosphorus pesticide ( diazinon, parathion- methyl, pirimiphos- methyl, isocarbophos and quinalphos) in environmental water samplesprior to Gas Chromatography ( GC) detection. The method, which took the advantages of both high adsorption capacity of graphene and easy separation fromthe sample solution of Fe3O4, could avoid the time- consuming experimental procedures commonly involved in the traditional solid phase extraction such as centrifugation and filtrations.Various experimental parameters affecting the extraction efficiencies such as the amount of the magnetic nanocomposite, extraction time, salt concentration, and desorption conditions were investigated.The optimal adsorbent dosage was 20 mg, and the most appropriate extraction time was 15 min, and the most suitable salt concentration was 0.5%.What's more, the ideal elution was acetonitrile and 1.5m L was chosen as the elution volume.Under the optimum conditions, the linear correlation coefficient ranged from 0.9985 to0.9996.The limits of detection of the method were between 0.0002 and 0.009 ng / m L, the relative standard deviations ( RSDs) for five replicates ranged from 3.2% to 7.8%. The results indicated that as a magnetic solid-phaseextraction adsorbent, the graphene- ferriferrous oxide ( G- Fe3O4) had a great potential for the preconcentration of pesticides from liquid samples.
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[1] Mirka, Ivo.Magnetic solid-phase extraction[J].Journal of Magnetism and Magnetic Materials, 1999, 194 (1) :108-112.
[2] Ajeet K, Pratima R S, Anees A A, et al.Chitosaniron-oxide nanobiocomposite based immunosensor for ochratoxin-A[J].Electrochemistry Communications, 2008, 10 (9) :1364-1368.
[3] Shaoqing S, Richuan R, Hongxiao Y, et al.Facile synthesis of Fe3O4/MWCNTs by spontaneous redox and their catalytic performance[J].Nanotechnology, 2010, 21 (18) :185602-185607.
[4] Hongmei S, Linyuan C, Lehui L.Magnetite/reduced graphene oxide nanocomposites:one step solvothermal synthesis and use as a novel platform for removal of dye pollutants[J].Nano Research, 2011, 4 (6) :550-562.
[5] Matthew J A, Vincent C T, Richard B K.Honeycomb carbon:A review on graphene[J].Chemical Reviews, 2010, 110 (1) :132-145.
[6] Dreyer D R, Park S, Bielawski C W, et al.The chemistry of graphene oxide[J].Chemical Society Reviews, 2010, 39 (1) :228-240.
[7] Luo Y B, Shi Z G, Gao Q, et al.Magnetic retrieval of graphene:extraction of sulfonamide antibiotics from environmental water samples[J].Journal of Chromatography A, 2011, 1218 (10) :1353-1358.
[8] Chandra V, Park J, Chun Y, et al.Water-dispersible magnetite-reduced graphene oxide composites for arsenic removal[J].Acs Nano, 2010, 4 (7) :3979-3986.
[9] Nianwu L, Mingbo Z, Xiaofeng C, et al.Preparation of magnetic Co Fe2O4-functionalized graphene sheets via a facile hydrothermal method and their adsorption properties, 2011, 184 (4) :953-958.
[10] 余晟, 黄克靖, 余萌, 等.固相萃取-高效液相色谱法同时检测水样中戊唑醇、乙霉威、晴菌唑、精甲霜灵和扑草净5种农药残留[J].分析化学, 2012, 40 (7) :1065-1070. [11] 谢洪学, 何丽君, 吴秀玲, 等.分散液液微萃取-气相色谱法测定水样中甲拌磷农药[J].分析化学, 2008, 36 (11) :1543-1546. [12] 周欣, 臧晓欢, 王东跃, 等.分散液液微萃取-气相色谱联用测定葡萄中百菌清、克菌丹和灭菌丹的残留[J].分析化学, 2009, 37 (1) :41-45. [13] Weina W, Xiaoxing M, Qiuhua W, et al.The use of graphene-based magnetic nanoparticles as adsorbent for the extraction of triazole fungicides from environmental water[J].Journal of Separation Science, 2012, 35 (17) :2266-2272.
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