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Simultaneous detection of residues of 34 beta-lactam antibiotics in livestock and fish samples through liquid chromatography-tandem mass spectrometry

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Abstract

β-Lactam is one of the widely used veterinary drugs, but simultaneous analytical methods for β-lactam on various animal foods have not been established. In this study, we aimed to detect 34 β-lactam antibiotics simultaneously in livestock samples (beef, pork, chicken, egg, and milk) by liquid chromatography-tandem mass spectrometry (LC–MS/MS). Samples were extracted using phosphate buffer/acetonitrile or water/acetonitrile and then cleaned with 150 mg of C18 and 900 mg of MgSO4. The method showed acceptable recovery and repeatability of 66.1–119% and 1.5–26%, respectively. The method was employed to monitor 127 real samples from the domestic market to confirm its applicability, and no β-lactam residues were detected. It was also applied to other matrices (eel, flat fish, and shrimp) and showed acceptable recovery (62.1–120%) and repeatability (1.0–28%). The method is expected to improve the efficiency of monitoring veterinary drug residues in domestic livestock products and fishery foods.

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References

  • Bessaire T, Mujahid C, Beck A, Tarres A, Savoy MC, Woo PM, Mottier P, Desmarchel A. Screening of 23 β-lactams in foodstuffs by LC–MS/MS using an alkaline QuEChERS-like extraction. Food Additives & Contaminants: Part A. 35: 661-673 (2018)

    CAS  Google Scholar 

  • Bush K, Bradford PA. β-Lactams and β-lactamase inhibitors: An overview. Cold Spring Harbor Perspectives in Medicine. 6: 1-22 (2014)

    Google Scholar 

  • Carlson M, Thompson RD. Analyte loss due to membrane filter adsorption as determined by high-performance liquid chromatography. Journal of Chromatographic Science. 38: 77-83 (2000)

    Article  CAS  PubMed  Google Scholar 

  • Cámara M, Gallego-Picó A, Garcinuño RM, Fernández-Hernando P, Durand-Alegría JS, Sánchez PJ. An HPLC-DAD method for the simultaneous determination of nine β-lactam antibiotics in ewe milk. Food Chemistry. 141: 829-834 (2013)

    Article  PubMed  Google Scholar 

  • Cañada-Cañada F, Peña AM, Espinosa-Mansilla A. Analysis of antibiotics in fish samples. Analytical and Bioanalytical Chemistry. 395: 987-1008 (2009)

    Article  PubMed  Google Scholar 

  • Chaudhry SB, Veve MP, Wagner JL. Cephalosporins: A focus on side chains and β-lactam cross-reactivity. Pharmacy. 7: 1-16 (2019)

    Article  Google Scholar 

  • Chen Q, Pan XD, Huang BF, Han JL. Quantification of 16 β-lactams in chicken muscle by QuEChERS extraction and UPLC-Q-Orbitrap-MS with parallel reaction monitoring. Journal of Pharmaceutical and Biomedical Analysis. 145: 525-530 (2017)

    Article  CAS  PubMed  Google Scholar 

  • Codex Alimentarius Commission. CAC/GL 71-2009 Guidelines for the design and implementation of national regulatory food safety assurance programme associated with the use of veterinary drugs in food producing animals (2009)

  • European Commission. (2008). www.emea.eu.int. Accessed Jan. 20, 2003.

  • Feng S, Chiesa OA, Kijak P, Chattopadhaya P, Lancaster V, Smith EA, Girard L, Sklenka S, Li H. Determination of ceftiofur metabolite desfuroylceftiofur cysteine disulfide in bovine tissues using liquid chromatography−tandem mass spectrometry as a surrogate marker residue for ceftiofur. Journal of Agricultural and Food Chemistry. 62: 5011-5019 (2014)

    Article  CAS  PubMed  Google Scholar 

  • Food Safety and Inspection Service (FSIS). CLG-BLAC.03: Screening and confirmation of β-lactam antibiotics by HPLC-MS/MS (2011)

  • Guidi LR, Santos FA, Ribeiro ACSR, Fernandes C, Silva LHM, Gloria MBA. A simple, fast and sensitive screening LC-ESI-MS/MS method for antibiotics in fish. Talanta. 163: 85-93 (2017)

    Article  CAS  PubMed  Google Scholar 

  • Heller DN, Nochetto CB, Rummel NG, Thomas MH. Development of multiclass methods for drug residues in eggs: hydrophilic solid-phase extraction cleanup and liquid chromatography/tandem mass spectrometry analysis of tetracycline, fluoroquinolone, sulfonamide, and β-lactam residues. Journal of Agricultural and Food Chemistry. 54: 5267-5278 (2006)

    Article  CAS  PubMed  Google Scholar 

  • Hornish RE, Hamlow PJ, Brown SA. Multilaboratory trial for determination of ceftiofur residues in bovine and swine kidney and muscle, and bovine milk. The Journal of AOAC International. 86: 30-38 (2003)

    Article  CAS  PubMed  Google Scholar 

  • Holstege DM, Puschner B, Whitehead G, Galey FD. Screening and mass spectral confirmation of β-lactam antibiotic residues in milk using LC-MS/MS. Journal of Agricultural and Food Chemistry. 50: 406-411 (2002)

    Article  CAS  PubMed  Google Scholar 

  • Jank L, Hoff RB, Tarouco PC, Barreto F, Pizzolato TM. β-Lactam antibiotics residues analysis in bovine milk by LC-ESI-MS/MS: a simple and fast liquid–liquid extraction method, Food Additives & Contaminants: Part A. 29: 497-507 (2012)

    Article  CAS  Google Scholar 

  • Jank L, Martins MT, Arsand JB, Hoff RB, Barreto F, Pizzolato TM. High-throughput method for the determination of residues of β-lactam antibiotics in bovine milk by LC-MS/MS. Food Additives & Contaminants: Part A. 32: 1992-2001 (2015)

    CAS  Google Scholar 

  • Jung Y, Kim D, Nam T, Seo D, Yoo M. Identification and quantification of multi-class veterinary drugs and their metabolites in beef using LC–MS/MS. Food Chemistry. 382(132313): 1-13 (2022)

    Article  Google Scholar 

  • Karageorgou E, Christoforidou S, Ioannidou M, Psomas E, Samouris G. Detection of β-lactams and chloramphenicol residues in raw milk-development and application of an HPLC-DAD method in comparison with microbial inhibition assays. Foods. 7(82): 1-12 (2018)

    Article  Google Scholar 

  • Ministry of Agriculture, Food and Rural Affairs (MAFRA). (2022). https://ebook.qia.go.kr/home/view.php?host=main&site=20230113_140444&listPageNow=0&list2PageNow=0&code=0&code2=0&code3=0&optionlisttype=L&searchcode=0&searchcode2=0&searchdate=0&searchkey=&searchval=&searchandor=&dummy=&&orders=. Accessed Jan. 13, 2023.

  • Ministry of Food and Drug Safety (MFDS). (2022). https://various.foodsafetykorea.go.kr/fsd/#/ext/Document/FC. Accessed Dec. 1, 2022.

  • Prescott JF. Chapter 9: Beta-lactam antibiotics: Cephalosporins. pp. 153-173. In: Antimicrobial therapy in veterinary medicine, 5th ed. John Wiley & Sons, Inc, Hoboken, New Jersey, USA (2013)

    Chapter  Google Scholar 

  • Rocco MD, Moloney M, O’Beirne T, Earley S, Berendsen B, Furey A, Danaher M. Development and validation of a quantitative confirmatory method for 30 β-lactam antibiotics in bovine muscle using liquid chromatography coupled to tandem mass spectrometry. Journal of Chromatography A. 1500: 121-135 (2017)

    Article  PubMed  Google Scholar 

  • Rezende CP, Almeida MP, Brito RB, Nonaka CK, Leite MO. Optimisation and validation of a quantitative and confirmatory LC-MS method for multi-residue analyses of β-lactam and tetracycline antibiotics in bovine muscle. Food additives and contaminants: Part A, chemistry, analysis, control, exposure and risk assessment. 29: 541-549 (2012)

    Article  CAS  Google Scholar 

  • Turnipseed SB, Storey JM, Lohne JJ, Andersen WC, Burger R, Johnson AS, Madson MR. Wide-scope screening method for multiclass veterinary drug residues in fish, shrimp, and eel using liquid chromatography-quadrupole high-resolution mass spectrometry. Journal of Agricultural and Food Chemistry. 65: 7252-7267 (2017)

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  • World Health Organization (WHO). Antimicrobial resistance: Global report on surveillance 2014 (2014)

Download references

Acknowledgements

This study was supported by a Grant (22191MFDS317) from the Ministry of Food and Drug Safety in 2022.

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Correspondence to Ji Young Kim.

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Park, S.Y., Kim, Y.R., Lim, S.J. et al. Simultaneous detection of residues of 34 beta-lactam antibiotics in livestock and fish samples through liquid chromatography-tandem mass spectrometry. Food Sci Biotechnol 33, 1467–1486 (2024). https://doi.org/10.1007/s10068-023-01405-y

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