食品科学 ›› 2026, Vol. 47 ›› Issue (16): 318-327.doi: 10.7506/spkx1002-6630-20260128-247

• 安全检测 • 上一篇    下一篇

烷氧基链调控的COF涂层搅拌棒用于果蔬农药残留高灵敏萃取与检测

付盈莹,柳作翎,段正超,王联芝   

  1. (湖北民族大学化学与环境工程学院,湖北?恩施 445000)
  • 出版日期:2026-08-25 发布日期:2026-09-03
  • 基金资助:
    国家自然科学基金地区科学基金项目(21267009;21262011)

Alkoxy Chain-Regulated COF-Coated Stir Bars for Highly Sensitive Extraction and Detection of Pesticide Residues in Fruits and Vegetables

FU Yingying, LIU Zuoling, DUAN Zhengchao, WANG Lianzhi   

  1. (School of Chemistry and Environmental Engineering, Hubei Minzu University, Enshi 445000, China)
  • Online:2026-08-25 Published:2026-09-03

摘要: 异菌脲、腐霉利和丙环唑是果蔬种植中常用的农药,其残留可能危害人体健康。本研究以3 种烷氧基修饰的对苯二甲醛衍生物(2,5-二甲氧基、2,5-二己氧基、2,5-二辛氧基)分别与1,3,5-三(4-氨基苯基)苯反应,合成了亚胺类共价有机框架材料(covalent organic frameworks,COFs),并将其分别命名为COF-a、COF-b和COF-c。通过物理黏附法将其涂覆于含铁芯玻璃棒表面,制备成搅拌棒用于富集水果中3 种农药残留。其中,COF-a因烷氧基链最短、空间位阻小、π-π相互作用强,对极性目标农药萃取效率最高且稳定性良好。基于此,建立了搅拌棒吸附萃取-高效液相色谱法同时检测3 种农药。该方法在1~1 000 μg/L范围内线性良好(R2≥0.991 8),检测限为0.21~0.52 μg/L。搅拌棒制备重现性良好,批内和批间相对标准偏差分别不超过5.6%和8.5%。应用于草莓和红果参样品,均未检出目标农药,加标回收率分别为81.4%~119%和86.2%~99.2%,表明该方法准确可靠,可为果蔬农残检测提供技术支持。

关键词: 共价有机框架;农药残留;搅拌棒吸附萃取;高效液相色谱;果蔬检测

Abstract: Iprodione, procymidone, and propiconazole are pesticides widely used in fruit and vegetable cultivation, and their residues may pose risks to human health. In this study, imine-linked covalent organic frameworks (COFs) were synthesized by reacting three alkoxy-modified terephthalaldehyde derivatives (2,5-dimethoxy, 2,5-dihexyloxy, and 2,5-dioctyloxy) with 1,3,5-tris(4-aminophenyl) benzene and they were named as COF-a, COF-b, and COF-c, respectively. These materials were physically coated onto iron-cored rods to prepare stir bars for the enrichment of the three pesticide residues in fruit samples. Among them, COF-a exhibited the highest extraction efficiency for the polar target pesticides due to its shortest alkoxy chain, minimal steric hindrance, and strong π-π interactions, along with good stability. Based on this, a stir bar sorptive extraction-high performance liquid chromatography (SBSE-HPLC) method was established for the simultaneous detection of iprodione, procymidone, and propiconazole. The method showed good linearity over the concentration range of 1–1 000 μg/L (determination coefficient R2 ≥ 0.991 8), with limits of detection (LOD) ranging from 0.21 to 0.52 μg/L. The prepared stir bars demonstrated good reproducibility, with inter- and intra-batch relative standard deviations (RSD) not exceeding 5.6% and 8.5%, respectively. Analysis of strawberry and Cyclocodon lancifolius fruit samples revealed no detectable target pesticide residues. Spiked recoveries ranged from 81.4% to 119% for strawberry and 86.2% to 99.2% for C. lancifolius fruit, indicating that the method is accurate and reliable for pesticide residue analysis in fruits and vegetables, offering technical support for food safety monitoring.

Key words: covalent organic frameworks; pesticide residues; stir bar sorptive extraction; high performance liquid chromatography; fruit and vegetable detection

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