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以Hummers法为基础,合成了磁性氨基化石墨烯(NH2-G/Fe3O4),用NH2-G/Fe3O4-Nafion修饰了玻碳电极,用于氯氟吡氧乙酸的固相微萃取处理,结合电化学发光技术(ECL),建立了高灵敏度检测环境中氯氟吡氧乙酸残留的分析方法。考察了吸附时间、溶液p H等相关参数对电化学发光强度的影响。在最优实验的条件下,体系的ECL猝灭值ΔI与氯氟吡氧乙酸的浓度的对数值在0.01~25μg/m L的范围内呈良好的线性关系(相关系数R2=0.9989),检出限(LOD)为3 ng/m L(S/N=3)。方法对玉米和河水样品的加标回收率分别为94.8%~104.3%和93.4%~103.2%,相对标准偏差分别为2.5%~4.5%和1.5%~5.7%。
Based on the Hummers method, a magnetically graphene oxide (NH2-G / Fe3O4) was synthesized. The glassy carbon electrode was modified with NH2-G / Fe3O4-Nafion for the solid-phase microextraction of fluroxypyr Electrochemiluminescence (ECL) was used to establish a method for the analysis of flurbiprofen residues in a highly sensitive assay environment. The effects of adsorption time, solution pH and other parameters on the chemiluminescence intensity were investigated. Under optimal conditions, the linear relationship between the ECL quenching value ΔI and the logarithm of the concentration of fludizine in the range of 0.01-25 μg / m L (correlation coefficient R2 = 0.9989) The LOD was 3 ng / m L (S / N = 3). The spiked recoveries of corn and river water samples were 94.8% -104.3% and 93.4% -103.2%, respectively, and the relative standard deviations were 2.5% -4.5% and 1.5% -5.7%, respectively.