An optimized SPE-UPLC-MS/MS method for simultaneous quantification of 11 tetracyclines in dairy products
文献类型： 外文期刊
作者： Gao, Pengfei 1 ; Yin, Boxing 3 ; Yang, Renqin 3 ; Hong, Yiwei 4 ; Cao, Yang 4 ; Guo, Yawen 4 ; Ding, Hao 1 ; Xu, Junjie 4 ; Hong, Lu 4 ; Cai, Jingjing 4 ; Cheng, Sihui 4 ; Zhang, Genxi 4 ; Guo, Xiaodong 4 ; Xie, Xing 2 ; Xie, Kaizhou 1 ;
作者机构： 1.Yangzhou Univ, Coll Vet Med, Yangzhou, Peoples R China
2.Jiangsu Acad Agr Sci, Inst Vet Med, Key Lab Vet Biol Engn & Technol, Minist Agr, Nanjing 210014, Peoples R China
3.Yangzhou Univ, Expt Farm, Yangzhou, Peoples R China
4.Yangzhou Univ, Coll Anim Sci & Technol, Joint Int Res Lab Agr & Agriprod Safety, Yangzhou 225009, Peoples R China
关键词： tetracycline antibiotics; veterinary drug residues; milk safety; UPLC-MS/MS; multi-residue analysis
期刊名称：JOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE （ 影响因子：3.5； 五年影响因子：4.2 ）
ISSN： 0022-5142
年卷期： 2025 年
页码：
收录情况： SCI
摘要： 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 Na(2)EDTA-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) C-18 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 mu g kg(-1) and 0.07-2.78 mu g 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. (c) 2025 Society of Chemical Industry.
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