食品科学 ›› 2021, Vol. 42 ›› Issue (4): 297-304.doi: 10.7506/spkx1002-6630-20200627-343

• 安全检测 • 上一篇    下一篇

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

连玉晶,周一冉,孙欣,陈佳楠,郑振佳,王明林   

  1. (山东农业大学食品科学与工程学院,山东?泰安 271018)
  • 出版日期:2021-02-25 发布日期:2021-02-25
  • 基金资助:
    “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

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

LIAN Yujing, ZHOU Yiran, SUN Xin, CHEN Jianan, ZHENG Zhenjia, WANG Minglin   

  1. (College of Food Science and Engineering, Shandong Agricultural University, Tai’an 271018, China)
  • Online:2021-02-25 Published:2021-02-25

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。

关键词: QuEChERS;农药残留;磁性纳米粒子;净化

Abstract: 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.

Key words: QuEChERS; pesticide residues; magnetic nanoparticles; clean-up

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