基于胺基功能化磁性纳米粒子改进QuEChERS方法结合GC-MS/MS检测果蔬中7种农药残留  

Development of a Modified QuEChERS Method Based on Amine-Functionalized Iron Oxide Nanoparticles for the Simultaneous Determination of Seven Pesticides in Fruits and Vegetables by GC-MS/MS

作　　者：连玉晶[1] 周一冉 孙欣[1] 陈佳楠 郑振佳[1] 王明林[1] LIAN Yujing;ZHOU Yiran;SUN Xin;CHEN Jianan;ZHENG Zhenjia;WANG Minglin(College of Food Science and Engineering,Shandong Agricultural University,Tai’an 271018,China)

机构地区：[1]山东农业大学食品科学与工程学院,山东泰安271018

出　　处：《食品科学》2021年第4期297-304,共8页Food Science

基　　金：“十三五”国家重点研发计划重点专项(2018YFC1602300);山东省2018年度农业重大应用技术创新项目。

摘　　要：为简化QuEChERS方法并提高净化效果,通过化学共沉淀法及硅烷化反应,制备3-[2-(2-氨基乙基氨基)乙基氨基]丙基功能化四氧化三铁(3-[2-(2-aminoethylamino)ethylamino]propyltrimethoxy functional iron oxide,Fe3O4@SiO2-PAAA)磁性纳米粒子。并通过透射电子显微镜、傅里叶变换红外光谱、振动样品磁强计、X射线光电子能谱和Zeta电位分析对其进行表征。以Fe3O4@SiO2-PAAA作为吸附剂改进QuEChERS方法,结合气相色谱-串联质谱检测果蔬中7种农药残留。在最佳条件下,目标分析物在0.007~1.000 mg/kg质量浓度之间呈线性关系,相关系数(r2)大于0.994;该方法的定量限在0.007~0.017 mg/kg之间;在以定量限、2倍定量限和10倍定量限3个水平的添加回收率实验中,目标物的回收率在75.2%~105.4%范围内;相对标准偏差在3.7%~15.7%之间。该方法快速、准确、高效和灵敏,可作为果蔬中农药多残留分析的参考方法。In this study,3-[2-(2-aminoethylamino)ethylamino]propyltrimethoxy functional iron oxide(Fe3O4@SiO2-PAAA)magnetic nanoparticles(MNPs)were prepared by a chemical co-precipitation method and silanization reaction and used to simplify the QuEChERS(Quick,Easy,Cheap,Effective,Rugged,and Safe)method and simultaneously improve the purification efficiency.MNPs were characterized by transmission electron microscopy,Fourier transform infrared spectroscopy,vibrating sample magnetometry,X-ray photoelectron spectroscopy,and zeta potential analysis.A modified QuEChERS method was developed using Fe3O4@SiO2-PAAA as an adsorbent for detecting seven pesticide residues in fruits and vegetables using gas chromatography-tandem mass spectrometry(GC-MS/MS).Under the optimized conditions,the developed method showed a good linear relationship in the concentration range between 0.007 and 1.000 mg/kg with correlation coefficients(r2)above 0.994.The limits of quantitation(LOQs)for the method were between 0.007 and 0.017 mg/kg.At LOQ,2 LOQ,and 10 LOQ fortification levels,the recoveries were in the range from 75.2%to 105.4%for the seven pesticides,with relative standard deviations(RSDs)between 3.7%and 15.7%.This method is fast,accurate,effective and sensitive,and can be used as a reference method for the analysis of pesticide residues in fruits and vegetables.

关 键 词：QUECHERS 农药残留 磁性纳米粒子 净化 

分 类 号：TS207.3[轻工技术与工程—食品科学]