Cao Xiaolin, Jiang Zejun, Wang Shanshan, Hong Sihui, Li Hui, Shao Yong, She Yongxin, Wang Jing, Jin Fen, Jin Maojun
Key Laboratory of Agri-Food Safety and Quality, Institute of Quality Standard and Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing, P.R. China.
J Sep Sci. 2017 Dec;40(24):4747-4756. doi: 10.1002/jssc.201700674. Epub 2017 Dec 1.
Magnetic zeolitic imidazolate framework 67/graphene oxide composites were synthesized by one-pot method at room temperature for the first time. Electrostatic interactions between positively charged metal ions and both negatively charged graphene oxide and Fe O nanoparticles were expected to chemically stabilize magnetic composites to generate homogeneous magnetic products. The additional amount of graphene oxide and stirring time of graphene oxide, Co , and Fe O solution were investigated. The zeolitic imidazolate framework 67 and Fe O nanoparticles were uniformly attached on the surface of graphene oxide. The composites were applied to magnetic solid-phase extraction of five neonicotinoid insecticides in environmental water samples. The main experimental parameters such as amount of added magnetic composites, extraction pH, ionic strength, and desorption solvent were optimized to increase the capacity of adsorbing neonicotinoid insecticides. The results show limits of detection at signal-to-noise ratio of 3 were 0.06-1.0 ng/mL under optimal conditions. All analytes exhibited good linearity with correlation coefficients of higher than 0.9915. The relative standard deviations for five neonicotinoid insecticides in environmental samples ranged from 1.8 to 16.5%, and good recoveries from 83.5 to 117.0% were obtained, indicating that magnetic zeolitic imidazolate framework 67/graphene oxide composites were feasible for analysis of trace analytes in environmental water samples.
首次在室温下通过一锅法合成了磁性沸石咪唑酯骨架67/氧化石墨烯复合材料。预计带正电荷的金属离子与带负电荷的氧化石墨烯和Fe₃O₄纳米颗粒之间的静电相互作用能够化学稳定磁性复合材料,从而生成均匀的磁性产物。研究了氧化石墨烯的额外用量以及氧化石墨烯、Co²⁺和Fe₃O₄溶液的搅拌时间。沸石咪唑酯骨架67和Fe₃O₄纳米颗粒均匀地附着在氧化石墨烯表面。将该复合材料应用于环境水样中5种新烟碱类杀虫剂的磁性固相萃取。对添加磁性复合材料的量、萃取pH值、离子强度和解吸溶剂等主要实验参数进行了优化,以提高吸附新烟碱类杀虫剂的能力。结果表明,在最佳条件下,信噪比为3时的检测限为0.06 - 1.0 ng/mL。所有分析物均表现出良好的线性,相关系数高于0.9915。环境样品中5种新烟碱类杀虫剂的相对标准偏差在1.8%至16.5%之间,回收率在83.5%至117.0%之间,表明磁性沸石咪唑酯骨架67/氧化石墨烯复合材料可用于分析环境水样中的痕量分析物。