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采用适配体功能化 Fe O /氧化石墨烯磁性固相萃取 HPLC 法测定蜂蜜和牛奶中的氯霉素。

Determination of Chloramphenicol in Honey and Milk by HPLC Coupled with Aptamer-Functionalized Fe O /Graphene Oxide Magnetic Solid-Phase Extraction.

机构信息

College of Chemistry and Life Sciences, Zhejiang Normal Univ., Jinhua, 321004, China.

College of Geography and Environmental Sciences, Zhejiang Normal Univ., Jinhua, 321004, China.

出版信息

J Food Sci. 2019 Dec;84(12):3624-3633. doi: 10.1111/1750-3841.14955. Epub 2019 Nov 24.

DOI:10.1111/1750-3841.14955
PMID:31762030
Abstract

An aptamer-functionalized Fe O /graphene oxide was synthesized by chemical co-precipitation method and then employed in the magnetic solid-phase extraction for selective enrichment of chloramphenicol before HPLC. The aptamer was covalently bonded to the Fe O /graphene oxide complex by 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride and N-hydroxysuccinimide. Parameters affecting extraction efficiency including solution pH, extraction time and temperature, types and volume of elution solvent, and elution time were investigated in detail. Under the optimal conditions, good linearity was obtained between the peak area and analyte concentration in the range of 7.0 to 1.0 × 10  µg/L with the correlation coefficient of 0.9994. The limit of detection and quantitation were 0.24 µg/L and 0.79 µg/L, respectively. The developed method was employed to the analysis of chloramphenicol in honey and milk samples. The recoveries ranged from 80.5% to 105.0% with relative standard deviations less than 8.9%. PRACTICAL APPLICATION: An aptamer-functionalized Fe O /graphene oxide was synthesized and employed in magnetic solid phase extraction for the enrichment of chloramphenicol before HPLC. The presented assay was employed for the determination of chloramphenicol in honey and milk with satisfactory results.

摘要

一种适配子功能化的 Fe3O4/氧化石墨烯通过化学共沉淀法合成,并用于高效液相色谱前磁性固相萃取选择性富集氯霉素。适配子通过 1-乙基-3-(3-二甲基氨基丙基)碳化二亚胺盐酸盐和 N-羟基琥珀酰亚胺共价键合到 Fe3O4/氧化石墨烯复合物上。详细研究了影响萃取效率的参数,包括溶液 pH 值、萃取时间和温度、洗脱溶剂的类型和体积以及洗脱时间。在最佳条件下,在 7.0 至 1.0×10-2µg/L 范围内,峰面积与分析物浓度之间呈良好线性关系,相关系数为 0.9994。检测限和定量限分别为 0.24µg/L 和 0.79µg/L。该方法用于蜂蜜和牛奶样品中氯霉素的分析。回收率在 80.5%至 105.0%之间,相对标准偏差小于 8.9%。实际应用:合成了一种适配子功能化的 Fe3O4/氧化石墨烯,并用于高效液相色谱前磁性固相萃取富集氯霉素。该方法用于测定蜂蜜和牛奶中的氯霉素,结果令人满意。

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