中文摘要：本文采用正负电极自组装方法制备了一种新型磁性聚乙烯亚胺修饰还原氧化石墨烯，采用透射电子显微镜（TEM），傅里叶变换红外光谱（FT-IR）、X-射线衍射（XRD）、热重分析仪（TGA）、振动样品磁强计（VSM）和Zeta电位分析等方法对其进行了表征，并与高效液相色谱法联用成功地对大米中四苯羧酸类除草剂和麦草畏农药残留进行了检测。与Fe3O4@PEI、Fe3O4/RGO 和Fe3O4@PEI-GO相比，本文所制备的Fe3O4@PEI-RGO固体磁性吸附剂集成了PEI和 RGO的特性，具有更高的极性酸性除草剂提取效率且吸附机制更好。最佳条件下，校准曲线浓度范围为2μg/g -300μg/g，相关系数在0.9985-0.9994之间，检测限范围为0.67μg/g -2μg/g，回收率为87.41%-102.52%，相对标准差小于8.94%。因此，本研究建立的磁性聚乙烯亚胺修饰还原氧化石墨烯吸附技术是一种高效的预处理和富集方法，能对复杂基质中的极性酸性除草剂进行特异性萃取和检测。
外文摘要：A novel magnetic polyethyleneimine modified reduced graphene oxide (Fe3O4@PEI-RGO) had been fabricated based on a self-assemble approach between positive charged magnetic polyethyleneimine (Fe3O4@PEI) and negative charged GO sheets via electrostatic interaction followed by chemical reduction of GO to RGO. The as-prepared Fe3O4@PEI-RGO was characterized by transmission electron microscopy (TEM), Fourier transform infrared spectrometry (FT-IR), X-ray diffraction (XRD), thermal gravimetric analyzer (TGA), vibrating sample magnetometer (VSM) and zeta potential analysis, and then was successfully applied to determine four phenoxy acid herbicides and dicamba in rice coupled with high performance liquid chromatography (HPLC). As a surface modifier of RGO, PEI not only effectually affected the surface property of RGO (e.g. zeta potential), but also changed the polarity of RGO and offered anion exchange groups to polar acidic herbicides, which would directly influence the type of adsorbed analytes. Compared with Fe3O4@PEI, Fe3O4/RGO and Fe3O4@PEI-GO, the as-prepared Fe3O4@PEI-RGO, integrating the superiority of PEI and RGO, showed higher extraction efficiency for polar acidic herbicides. Besides, the adsorption mechanism was investigated as well. It turned out that electrostatic interaction and p-p interaction were considered to be two major driving force for the adsorption process. Response surface methodology (RSM), a multivariate experimental design technique, was used to optimize experimental parameters affecting the extraction efficiency in detail. Under the optimal conditions, a satisfactory performance was obtained. The calibration curves were linear over the concentration ranging from 2 to 300 ng g(-1) with correlation coefficients (r) between 0.9985 and 0.9994. The limits of detection (LODs) were in the range of 0.67-2 ng g(-1). The recoveries ranged from 87.41% to 102.52% with relative standard deviations (RSDs) less than 8.94%. Taken together, the proposed method was an efficient pretreatment and enrichment procedure and could be successfully applied for selective extraction and determination of polar cidic herbicides in complex matrices. (C) 2016 Elsevier B.V. All rights reserved.
外文关键词：vegetables, pesticide residues, health risk, hazard index, hazard quotient
作者：Li, Na; Chen, Juan; Shi, Yan-Ping
作者单位：Chinese Acad Sci, Key Lab Chem Northwestern Plant Resources, Lanzhou 730000, Peoples R China.
期刊名称：ANALYTICA CHIMICA ACTA
期刊影响因子：4.712
出版年份：2017
出版刊次：1
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