食品科学 ›› 2026, Vol. 47 ›› Issue (18): 323-330.doi: 10.7506/spkx1002-6630-20260305-035

• 安全检测 • 上一篇    

电场强化ZIF-8/碳布膜萃取-高效液相色谱法测定牛奶、蜂蜜中四环素类抗生素残留

杨 成1,孙嵇成1,张国强2,庞月红1,沈晓芳1,*   

  1. (1.江南大学食品学院,江苏 无锡 214122;2.山西晋恒检测科技有限公司,山西 太原 030032)
  • 发布日期:2026-09-29
  • 基金资助:
    “十四五”国家重点研发计划重点专项(2022YFF1100803); 食品药品安全防控山西省重点实验室项目(202204010931006)

Electric Field-Enhanced ZIF-8/Carbon Cloth Membrane Extraction Coupled with High Performance Liquid Chromatography for Determination of Tetracycline Antibiotics in Milk and Honey

YANG Cheng, SUN Jicheng, ZHANG Guoqiang, PANG Yuehong, SHEN Xiaofang   

  1. (1. School of Food Science and Technology, Jiangnan University, Wuxi 214122, China;2. Shanxi Jinheng Testing Technology Co. Ltd., Taiyuan 030032, China)
  • Published:2026-09-29

摘要: 通过将金属有机骨架材料ZIF-8原位生长于碳布表面,制备电场增强-薄膜微萃取电极,结合高效液相色谱,建立一种用于四环素类抗生素(土霉素、四环素和强力霉素)快速、高效、准确的分析方法,并将其应用于动物源食品(蜂蜜和牛奶)中目标抗生素的萃取与检测。利用扫描电子显微镜、傅里叶变换红外光谱和N2吸附-脱附等温线对ZIF-8/碳布的形貌、结构及吸附性能进行表征。结果表明,所制备材料具有良好的吸附特性。在最佳条件下,所建立的方法可以在20 min达到萃取平衡。在最优前处理条件下,本方法在8.0~200.0 ng/mL质量浓度范围内,3 种四环素类抗生素均呈现良好的线性关系(R2>0.992),检出限和定量限(limits of quantification,LOQ)分别为2.0~2.5 ng/mL和8.0~8.5 ng/mL。在实际样品蜂蜜和牛奶的检测中,强力霉素在两种牛奶样品中均有痕量检出(<LOQ),加标量为20、50 ng/g与100 ng/g时的回收率为81.5%~103.0%,相对标准偏差(n=5)均不大于7.2%。本研究开发的基于ZIF-8/碳布的电场增强-薄膜微萃取可用于动物源食品中四环素类抗生素的检测,为食品安全监管提供一种有效的样品前处理手段。

关键词: 薄膜微萃取;电场增强;高效液相色谱;碳布;四环素类抗生素

Abstract: By in situ growing the metal-organic framework ZIF-8 on the surface of carbon cloth (CC), an electric field-enhanced thin-film microextraction (EE-TFME) electrode was prepared and combined with high performance liquid chromatography (HPLC) to develop a rapid and accurate analytical method for the determination of tetracycline antibiotics (oxytetracycline, tetracycline, and doxycycline) in animal-derived food products (honey and milk). The morphology, structure, and adsorption properties of ZIF-8/CC were characterized by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, and N2 adsorption-desorption isotherms. The results indicated that the prepared material exhibited favorable adsorption characteristics. Under optimal conditions, the developed method achieved extraction equilibrium within 20 min. It showed good linearity for the three tetracycline antibiotics in the concentration range of 8.0-200.0 ng/mL (R2 > 0.992). The limits of detection (LOD) and quantification (LOQ) were 2.0-2.5 and 8.0-8.5 ng/mL, respectively. In honey and milk samples, doxycycline was detected at trace levels (< LOQ). At spiked concentrations of 20, 50 and 100 ng/g, recoveries ranged from 81.5% to 103.0%, with relative standard deviations (RSD, n = 5) no more than 7.2%. The EE-TFME method based on ZIF-8/carbon cloth developed in this study can be applied to the detection of tetracycline antibiotics in animal-derived foods, providing an effective sample pretreatment approach for food safety monitoring.

Key words: thin-film microextraction; electric field-enhanced; high performance liquid chromatography; carbon cloth; tetracycline antibiotics

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