色谱

色谱 ›› 2021, Vol. 39 ›› Issue (4): 349-356.DOI: 10.3724/SP.J.1123.2020.12012

• 研究快报 • 上一篇    下一篇

基于室温溶液悬浮法共价有机骨架的制备及其对茶叶中拟除虫菊酯固相微萃取的应用

余奇东1, 张兰2,*(), 张文敏3, 杨江帆1,*()   

  1. 1.福建农林大学园艺学院, 福建 福州 350002
    2.福州大学, 食品安全与生物分析教育部重点实验室, 福建 福州 350116
    3.闽江师范高等专科学校, 化学与生物工程系, 福建 福州 350108
  • 收稿日期:2020-12-10 出版日期:2021-04-08 发布日期:2021-03-08
  • 通讯作者: 张兰,杨江帆
  • 作者简介:E-mail: zlan@fzu.edu.cn(张兰).
    *E-mail: yjf3001@163.com(杨江帆);
  • 基金资助:
    福建省“2011协同创新中心”中国乌龙茶产业协同创新中心专项(J2015-75)

Preparation of covalent organic framework based on room temperature solution-suspension approach and its application to solid-phase microextraction of pyrethroids in tea

YU Qidong1, ZHANG Lan2,*(), ZHANG Wenmin3, YANG Jiangfan1,*()   

  1. 1. College of Horticulture, Fujian Agriculture and Forestry University, Fuzhou 350002, China
    2. Ministry ofEducation Key Laboratory of Analytical Science of Food Safety and Biology, Fuzhou University, Fuzhou 350116,China
    3. Division of Chemical and Biological Engineering, Minjiang Teachers College, Fuzhou 350108, China
  • Received:2020-12-10 Online:2021-04-08 Published:2021-03-08
  • Contact: ZHANG Lan,YANG Jiangfan
  • Supported by:
    Collaborative Innovation Center of Chinese Oolong Tea Industry-Collabortive Innovation Center (2011) of Fujian Province(J2015-75)

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摘要：

拟除虫菊酯(PYs)类农药被广泛用于茶园病虫害的防治。随着国内外对进出口茶叶中农药残留限量的要求日益严格,我国迫切地需要开发能应用于检测茶叶中痕量PYs的方法。研究通过简单、温和的溶液悬浮法(SSA),在室温下制备了共价有机骨架(COF)材料TpBD,该材料具有优异的热/化学稳定性、较高的孔隙度和比表面积。通过简单物理黏附的方法,将TpBD制备成固相微萃取(SPME)纤维。将准备好的纤维应用于固相微萃取技术并与气相色谱-串联质谱(GC-MS/MS)联用,建立用于检测PYs的高灵敏分析方法。该方法对氟氯氰菊酯、氯氰菊酯、氟氰菊酯、氰戊菊酯和溴氰菊酯的富集倍数为702~2687,并表现出低的检出限(0.1~0.5 ng/L)、宽的线性范围(0.2~800 ng/L)、良好的线性关系(相关系数≥0.9991)、可接受的重复性(RSD≤11.0%, n=3)。将所建立的方法用于实际绿茶和乌龙茶样品中PYs残留量的检测,并成功地从实际茶样中检测出5种痕量PYs,并且具有满意的回收率(80.2%~109.5%)。实验结果表明,所建立的分析方法适用于茶叶中PYs农药残留量的分析和检测。此外,通过SSA成功地制备了TpBD材料,证实了该方法具有较好的普适性,具有简便合成其他COFs材料的潜力。

关键词: 气相色谱-串联质谱, 固相微萃取, 共价有机骨架材料, 拟除虫菊酯, 茶叶

Abstract:

Pyrethroids (PYs) have been widely used to control pests and prevent diseases in tea gardens. However, with the increasingly stringent pesticide testing standards in the import and export trade of tea, there is an urgent need for methods to detect trace amounts of PYs in tea. In this study, a covalent organic framework (COF) material TpBD with excellent thermal/chemical stability, high porosity, and a large specific surface area was prepared by a room-temperature solution-suspension approach (SSA). TpBD-coated solid phase microextraction (SPME) fibers were fabricated by coating the material on etched stainless-steel fibers by a simple physical coating method. The fibers were used in combination with gas chromatography-tandem mass spectrometry (GC-MS/MS) to establish a highly sensitive method for the detection of PYs. The enrichment factors of this method for cyfluthrin, cypermethrin, flucythrinate, fenvalerate, and deltamethrin were 702-2687. The method showed low LODs (0.1-0.5 ng/L), wide linear ranges (0.2-800 ng/L), good linearities (correlation coefficients (R)≥0.9991) and acceptable repeatabilities (RSD≤11.0%, n=3). Green tea and oolong tea samples were analyzed using the developed method, and trace levels of the five PYs were successfully detected. The recoveries of the spiked PYs in the real green tea and oolong tea samples were in the range of 80.2%-109.5%. Experimental results showed that the established analytical method is suitable for the determination of PY pesticides in tea. Furthermore, the TpBD material was successfully prepared by the SSA method, demonstrating that the method has good universality and excellent potential for the simple synthesis of other COF materials.

Key words: gas chromatography-tandem mass spectrometry (GC-MS/MS), solid phase microextraction (SPME), covalent organic frameworks (COFs), pyrethroids (PYs), tea

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