摘要
以磁性泡沫镍为基底制备泡沫镍基三维石墨烯磁固相萃取材料,建立磁固相萃取与气相色谱-电子捕获器联用技术用于鸡蛋中氟虫腈及其代谢物分析的新方法。将泡沫镍基三维石墨烯磁性材料用于磁固相萃取氟虫腈及其代谢物,萃取解吸条件如下:样品溶液盐浓度为30%,样品溶液pH为7,涡旋萃取5 min;解吸剂为乙腈,涡旋解吸5 min。采用气相色谱法进行定性定量分析。该方法对氟虫腈及其代谢物的检出限为4.1~5.9μg/L,线性范围为15~500μg/L,相关系数>0.9981。将所建方法用于鸡蛋样品检测,氟虫腈及其代谢物的加标回收率为83.3%~95.4%,相对标准偏差(n=3)为4.8%~11.7%。
In this work,nickel foam based three-dimensional graphene(3D/G)was prepared as the extraction material for magnetic solid phase extraction(MSPE).And a novel method of MSPE combined with gas chromatography-electron capture detection(GC-ECD)was established for the determination of fipronil and its metabolites in eggs.The extraction and desorption conditions of magnetic solid phase extraction were as follows:concentration of NaCl was 30%;sample pH was 7;vortex extraction for 5 min;desorption solvent was acetonitrile;vortex desorption for 5 min.Under the optimized conditions,the limits of detection(3S/N)were in the range of 4.1-5.9μg/L and the linear range of fipronil and its metabolites ranged from 15μg/L to 500μg/L with correlation coefficient(R)all above 0.9981.The proposed method was applied for the determination of fipronil and its metabolites in egg samples.The sample recoveries were in the range of 83.3%-95.4%with relative standard deviation(n=3)of 4.8%-11.7%.
作者
刘贝叶
杨波
蒲文权
杨文兵
卞超
马婷婷
范文莹
LIU Beiye;YANG Bo;PU Wenquan;YANG Wenbing;BIAN Chao;MA Tingting;FAN Wenying(Eighth Geological Brigade of Hubei Geological Bureau,Xiangyang 441000,China;School of Food Science and Technology,Hubei University of Arts and Science,Xiangyang 441053,China;College of Resource Environment and Tourism,Hubei University of Arts and Science,Xiangyang 441053,China)
出处
《中国测试》
CAS
北大核心
2023年第6期56-61,共6页
China Measurement & Test
基金
国家自然科学基金项目(42077143)
湖北省自然科学基金项目(2022CFD091)
2020年度湖北省地质八队科研计划项目(BDKY2020-10)
2020年湖北省高等学校优秀中青年科技创新团队计划项目(T2020016)
湖北文理学院2019年度教师科研能力培育基金自然科学类(2019KYPY001)。
关键词
三维石墨烯
泡沫镍
磁固相萃取
气相色谱
氟虫腈及其代谢物
3D graphene
nickel foam
magnetic solid phase extraction
gas chromatography
fipronil and its metabolites
