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合成COF(TAPA-DHTA)-海藻酸钠-钙聚丙烯酸酯复合微球作为吸附剂,用于在通过HPLC-MS/MS定量之前对食品和水中的氟喹诺酮类抗生素进行分散固相萃取。

Synthesis of COF (TAPA-DHTA)-sodium alginate-Ca-polyacrylate composite microspheres as adsorbent for dispersive solid phase extraction of fluoroquinolone antibiotics in food and water prior to the quantification by HPLC-MS/MS.

作者信息

Ao Rui, Xu Xiu-Li, Zhao Yanfang, Wang Jun, Hu Mei, Wang Xiu-Juan, Boukherroub Rabah, Chen Xiangfeng, Zhang Feng

机构信息

Shandong International Joint Laboratory of Environmental and Biological Science, Qilu University of Technology (Shandong Academy of Science), Jinan, Shandong, 250014, China; Institute of Food Safety, Chinese Academy of Quality and Inspection & Testing, Beijing 100176, China.

Institute of Food Safety, Chinese Academy of Quality and Inspection & Testing, Beijing 100176, China.

出版信息

J Chromatogr A. 2025 Aug 30;1757:466117. doi: 10.1016/j.chroma.2025.466117. Epub 2025 Jun 4.

Abstract

This work developed hydroxyl‑functionalized covalent organic framework (COF) via ambient-temperature synthesis and integrated it with sodium alginate-Ca²⁺-polyacrylate hydrogel to form composite microspheres (CACMPs) for dispersive solid-phase extraction (dSPE) of five fluoroquinolone antibiotics in milk , eggs and river water. Combining COF with hydrogel can effectively improve the hydrophilicity of adsorbent. The CACMPs do not require centrifugation and can be completely separated within one minute. After five cycles, they still maintain high extraction efficiency (>90 %). Coupled with HPLC-MS/MS, the method achieved a wide linear range (0.01-100 ng/mL), low detection limits (0.05-0.42 μg/kg), and high precision (RSD ≤20.5 %). Validation via spiked samples yielded recoveries of 80.3-117.3 %, confirming reliability for monitoring FQ residues in dairy. Design of CACMPs combines COF adsorption capacity with hydrogel practicality, offering a sustainable, efficient solution for antibiotic analysis in complex matrices.

摘要

本研究通过室温合成法制备了羟基功能化共价有机框架(COF),并将其与海藻酸钠-Ca²⁺-聚丙烯酸酯水凝胶相结合,形成复合微球(CACMPs),用于牛奶、鸡蛋和河水中五种氟喹诺酮类抗生素的分散固相萃取(dSPE)。将COF与水凝胶相结合能够有效提高吸附剂的亲水性。CACMPs无需离心,可在一分钟内完全分离。经过五个循环后,它们仍保持较高的萃取效率(>90%)。结合高效液相色谱-串联质谱(HPLC-MS/MS),该方法实现了宽线性范围(0.01-100 ng/mL)、低检测限(0.05-0.42 μg/kg)和高精度(RSD≤20.5%)。通过加标样品验证,回收率为80.3-117.3%,证实了该方法用于监测乳制品中氟喹诺酮残留的可靠性。CACMPs的设计将COF的吸附能力与水凝胶的实用性相结合,为复杂基质中抗生素分析提供了一种可持续、高效的解决方案。

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