An optimized SPE-UPLC-MS/MS method for simultaneous quantification of 11 tetracyclines in dairy products.

IF 3.5 2区农林科学 Q1 AGRICULTURE, MULTIDISCIPLINARY

Journal of the Science of Food and Agriculture Pub Date : 2025-07-29 DOI:10.1002/jsfa.70088

Pengfei Gao, Boxing Yin, Renqin Yang, Yiwei Hong, Yang Cao, Yawen Guo, Hao Ding, Junjie Xu, Lu Hong, Jingjing Cai, Sihui Cheng, Genxi Zhang, Xiaodong Guo, Xing Xie, Kaizhou Xie

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引用次数: 0

Abstract

Background: The global rise in antibiotic use, particularly tetracyclines (TCs) in animal husbandry, poses significant risks to food safety and public health due to residual accumulation and bacterial resistance. Existing detection methods for TCs in dairy products often lack efficiency, sensitivity, or the capability for simultaneous multi-residue analysis. Developing a rapid, precise, and cost-effective method to monitor TCs in compliance with international maximum residue limits remains an urgent need.

Results: We developed a streamlined approach integrating a three-step purification process (PRiME HLB cartridges) with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The method utilizes 0.1 mol L^-1 Na₂EDTA-McIlvaine buffer for extraction, achieving 83.11-107.61% recovery rates with < 5.43% relative standard deviation (RSD). Optimized chromatographic separation on a bridged ethyl-siloxane and silica hybrid (BEH) C₁₈ column enabled simultaneous detection of 11 TCs (including parent compounds and metabolites) within 9 min. Sensitivity was exceptional, with limits of detection and limits of quantification of 0.02-0.83 μg kg^-1 and 0.07-2.78 μg kg^-1, respectively. Intra-/inter-day precision (RSD 3.03-9.33%) and compliance with European Union/Food and Drug Administration (EU/FDA) were validated using real milk and milk powder samples.

Conclusions: This method combines rapid sample preparation with UPLC-MS/MS for simultaneous quantification of 11 TCs in dairy products. Its high accuracy, sensitivity, and compliance with global regulatory standards make it indispensable for large-scale food safety monitoring, effectively addressing antibiotic residue risks and supporting international trade harmonization. © 2025 Society of Chemical Industry.

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优化的SPE-UPLC-MS/MS同时定量乳制品中11种四环素的方法。

背景：全球抗生素使用的增加，特别是四环素类药物在畜牧业中的使用，由于残留积累和细菌耐药性，对食品安全和公众健康构成重大风险。现有的乳制品中TCs的检测方法往往缺乏效率、灵敏度或同时进行多残留分析的能力。开发一种符合国际最大残留限量的快速、精确和具有成本效益的方法来监测tc仍然是迫切需要的。结果：我们开发了一种简化的方法，将三步纯化过程（PRiME HLB试剂盒）与超高效液相色谱-串联质谱（UPLC-MS/MS）相结合。该方法采用0.1 mol L-1 Na2EDTA-McIlvaine缓冲液提取，在9 min内同时检测11种tc（包括母体化合物和代谢物），回收率为83.11-107.61%。灵敏度高，检测限为0.02 ~ 0.83 μg kg-1，定量限为0.07 ~ 2.78 μg kg-1。采用真实牛奶和奶粉样品验证日内/日间精密度（RSD 3.03-9.33%）和符合欧盟/食品药品监督管理局（EU/FDA）标准。结论：该方法将快速制样与UPLC-MS/MS相结合，可同时定量乳制品中11种总含量。其准确性、灵敏度高，且符合全球监管标准，是大规模食品安全监测、有效应对抗生素残留风险和支持国际贸易协调不可或缺的工具。©2025化学工业协会。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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来源期刊

Journal of the Science of Food and Agriculture 工程技术-农业综合

CiteScore

8.10

自引率

4.90%

发文量

634

审稿时长

3.1 months

期刊介绍： The Journal of the Science of Food and Agriculture publishes peer-reviewed original research, reviews, mini-reviews, perspectives and spotlights in these areas, with particular emphasis on interdisciplinary studies at the agriculture/ food interface. Published for SCI by John Wiley & Sons Ltd. SCI (Society of Chemical Industry) is a unique international forum where science meets business on independent, impartial ground. Anyone can join and current Members include consumers, business people, environmentalists, industrialists, farmers, and researchers. The Society offers a chance to share information between sectors as diverse as food and agriculture, pharmaceuticals, biotechnology, materials, chemicals, environmental science and safety. As well as organising educational events, SCI awards a number of prestigious honours and scholarships each year, publishes peer-reviewed journals, and provides Members with news from their sectors in the respected magazine, Chemistry & Industry . Originally established in London in 1881 and in New York in 1894, SCI is a registered charity with Members in over 70 countries.