食品科学 ›› 2017, Vol. 38 ›› Issue (18): 317-324.doi: 10.7506/spkx1002-6630-201718049

• 安全检测 • 上一篇    

多壁碳纳米管-聚醚砜复合膜净化法快速测定食品中15 种农药残留

何亚荟,王亮,王静   

  1. (1.信阳农林学院食品学院,河南?信阳 464000;2.中国农业科学研究院农业质量标准与检测技术研究所,北京 100081;3.神华地质勘查有限责任公司可燃冰研发办公室,北京 102211)
  • 出版日期:2017-09-25 发布日期:2017-09-04
  • 基金资助:
    河南省教育厅高等学校重点科研项目(17A550018);河南省科技攻关计划项目(172102310314)

Determination of 15 Pesticide Residues in Food Matrixes by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry after Sample Cleanup Using Polyethersulfone (PES)/Multiwalled Carbon Nanotubes (MWCNTs) Composite Membrane

HE Yahui, WANG Liang, WANG Jing   

  1. (1. Food College, Xinyang University of Agriculture and Forestry, Xinyang 464000, China; 2. Institute of Quality Standard and Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing 100811, China; 3. R&D Office of Methane Hydrate, Shenhua Geological Exploration Co. Ltd., Beijing 102211, China)
  • Online:2017-09-25 Published:2017-09-04

摘要: 采用相转化法,把吸附材料多壁碳纳米管填充到聚醚砜中,制备多壁碳纳米管-聚醚砜复合膜。由扫描电镜观察可知,复合膜呈指状孔结构。设计简便、易于操作的复合膜过滤前处理装置,将该复合膜和装置用于食品中农药多残留快速检测的前处理中,采用超高效液相色谱-串联质谱进行测定,建立食品中15?种农药的快速检测方法。结果显示:采用复合膜对样品进行快速前处理,净化效果良好,但由于复合膜中多壁碳纳米管的特殊平面环状结构,使得复合膜可能对平面型农药具有一定的吸附作用,15?种农药中,2?种平面型农药回收率不好,13?种非平面型农药的回收率平均值在71%~118%之间,相对标准偏差在0.73%~12.87%之间(n=6)。该方法使得整个样品前处理时间从4~7?h缩短到30?min内,并具有操作简单高效、灵敏度高、环境友好、易于普及的优点,适合于食品中非平面型农药残留的快速分析测定。

关键词: 多壁碳纳米管-聚醚砜复合膜, 食品, 农药残留, 超高效液相色谱-串联质谱, 测定

Abstract: In this paper, polyethersulfone (PES)/multi-walled carbon nanotubes (MWCNTs) composite membrane was prepared by phase inversion method, and its surface morphology and structure were observed by scanning electron microscopy (SEM). The results showed that the membrane displayed a finger-shaped porous structure. A simple, easy-to-operate filtration device equipped with the composite membrane was designed and used to develop a rapid sample pretreatment for the analysis of 15 pesticide residues in food by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Good sample cleanup was obtained with the composite membrane. However, due to the special planar ring structure of multi-walled carbon nanotubes incorporated in it, the composite membrane could adsorb planar pesticides. Consequently, of the 15 pesticides analyzed, the average recoveries of two planar pesticides were low while those of the other pesticides were between 71% and 118%, with relative standard deviation (RSD) between 0.73% and 12.87% (n = 6). The method reduced the overall sample preparation time from 4–7 h to 30 min. The method was simple, efficient, sensitive and environmentally friendly and could be applied widely. It was suitable for rapid analysis of non-planar pesticide residues in food.

Key words: polyethersulfone (PES)/multi-walled carbon nanotubes (MWCNTs) composite membrane, food, pesticide residues, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), determination

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