食品科学 ›› 2026, Vol. 47 ›› Issue (13): 323-333.doi: 10.7506/spkx1002-6630-20251105-035

• 安全检测 • 上一篇    下一篇

氨基多孔有机聚合物固相萃取结合高效液相色谱检测食品中氟喹诺酮类抗生素

向刚,黎文卓,赵小英,韦倩寒,陈志杨,李政,刘风平,黄青,彭金云   

  1. (1.广西民族师范学院化学与材料学院,崇左市锰资源综合利用技术重点实验室,广西锰资源高值化利用重点实验室,广西 崇左 532200;2.崇左市食品药品检验所,广西 崇左 532200)
  • 出版日期:2026-07-15 发布日期:2026-07-17
  • 基金资助:
    广西民族师范学院光电功能材料设计及其应用创新团队项目(KYTD202405); 广西民族师范学院校级科研项目(2024FW007;2025JB003);崇左市科技计划项目(20210719)

Determination of Fluoroquinolones in Foods by High Performance Liquid Chromatography Coupled with Solid-Phase Extraction Based on Amino Porous Organic Polymers

XIANG Gang, LI Wenzhuo, ZHAO Xiaoying, WEI Qianhan, CHEN Zhiyang, LI Zheng, LIU Fengping, HUANG Qing, PENG Jinyun   

  1. (1. Guangxi Key Laboratory for High-Value Utilization of Manganese Resources, Chongzuo Key Laboratory of Comprehensive Utilization Technology of Manganese Resources, College of Chemistry and Materials, Guangxi Minzu Normal University, Chongzuo 532200, China; 2. Chongzuo Institute for Food and Drug Control, Chongzuo 532200, China)
  • Online:2026-07-15 Published:2026-07-17

摘要: 以间苯二胺为单体,经FeCl3催化氧化聚合制备多孔有机聚合物(porous organic polymer,POP)-1,并对其结构及物理化学性质进行系统表征。将POP-1作为固相萃取(solid-phase extraction,SPE)吸附剂富集食品中的氟喹诺酮类抗生素,结合高效液相色谱(high performance liquid chromatography,HPLC)技术建立乳制品样品中氟喹诺酮类抗生素分析方法。结果表明,所制备材料由不规则球状固体相互联结而成,其表面尺寸不一的间隙构成多孔结构,比表面积和总孔容分别为3.99 m2/g与0.008 3 cm3/g。在样品前处理过程中,POP-1对氟喹诺酮类抗生素展现出优异的富集性能。乳制品样品中目标物的加标回收率为85.20%~119.15%,相对标准偏差为0.1%~7.9%,方法检出限为0.005 0~0.044 3 μg/L。综上,POP-1具有制备工艺简便、成本低廉、结构可设计性强及性能可调性优异等显著特点,基于此建立的SPE-HPLC分析方法兼具快速、简便优势,适用于乳制品中氟喹诺酮类抗生素的实际检测,该吸附剂具有良好的应用前景。

关键词: 氟喹诺酮类抗生素;多孔有机聚合物;固相萃取;吸附剂;高效液相色谱

Abstract: A porous organic polymer (POP)-1 was synthesized by the oxidative polymerization of m-phenylenediamine with FeCl3 as the oxidant and systematically characterized for its structure and physicochemical properties. The material was subsequently employed as a solid-phase extraction (SPE) sorbent for the enrichment of fluoroquinolone (FQ) antibiotics from foods. Furthermore, an analytical method based on SPE coupled with high performance liquid chromatography (HPLC) was established for the determination of FQ in milk. The results showed that POP-1 was formed by the interconnection of irregular spherical solids, and gaps of varying sizes on its surface formed a porous structure, with a specific surface area and total pore volume of 3.99 m2/g and 0.008 3 cm3/g, respectively. During sample pretreatment, POP-1 exhibited outstanding affinity for FQ antibiotics. Recoveries for spiked dairy products ranged from 85.20% to 119.15% with relative standard deviations of 0.1%–7.9%. Limits of detection were 0.005 0–0.044 3 μg/L. In conclusion, POP-1 offers distinct advantages including simple preparation, low cost, strong structural designability, and excellent performance tunability, showing promising application prospects. The developed SPE-HPLC method is rapid, straightforward, and suitable for the practical detection of FQ antibiotics in dairy products.

Key words: fluoroquinolone antibiotics; porous organic polymers; solid-phase extraction; sorbents; high performance liquid chromatography

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