{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,1,22]],"date-time":"2026-01-22T10:44:47Z","timestamp":1769078687035,"version":"3.49.0"},"reference-count":25,"publisher":"MDPI AG","issue":"1","license":[{"start":{"date-parts":[[2015,12,24]],"date-time":"2015-12-24T00:00:00Z","timestamp":1450915200000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Antibiotics"],"abstract":"<jats:p>The use of medicated feed is a common practice in animal food production to improve animal health. Tetracyclines and \u03b2-Lactams are the groups that are most frequently added to this type of feed. The measurement of the concentration of the analytes in these types of samples is sometimes due to the matrix characteristic, and manufacturers are demanding fast, precise and reproducible methods. A rapid confirmatory method based on a simple extraction protocol using acidified methanol and followed by high performance liquid chromatography coupled to a tandem mass spectrometer for the quantification of four tetracyclines in feed is presented. Validation was performed following the guidelines of Decision 2002\/657\/EC. Results indicated that the four tetracyclines can be identified and quantified in a concentration range between 50 and 500 mg\/kg with recoveries between 84% and 109% and RSD for precision under reproducible conditions between 12% and 16%. Satisfactory results were also obtained with interlaboratory studies and by comparing the method with an HPLC-Fluorescent method.<\/jats:p>","DOI":"10.3390\/antibiotics5010001","type":"journal-article","created":{"date-parts":[[2015,12,24]],"date-time":"2015-12-24T10:03:53Z","timestamp":1450951433000},"page":"1","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":21,"title":["Analysis of Tetracyclines in Medicated Feed for Food Animal Production by HPLC-MS\/MS"],"prefix":"10.3390","volume":"5","author":[{"given":"Rosa","family":"Gavil\u00e1n","sequence":"first","affiliation":[{"name":"Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Veterinary Medicine, University of Santiago de Compostela, 27002 Lugo, Spain"}]},{"given":"Carolina","family":"Nebot","sequence":"additional","affiliation":[{"name":"Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Veterinary Medicine, University of Santiago de Compostela, 27002 Lugo, Spain"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7992-1491","authenticated-orcid":false,"given":"Jose","family":"Miranda","sequence":"additional","affiliation":[{"name":"Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Veterinary Medicine, University of Santiago de Compostela, 27002 Lugo, Spain"}]},{"given":"Yolanda","family":"Mart\u00edn-G\u00f3mez","sequence":"additional","affiliation":[{"name":"Laboratorio de Sanidad Animal, Lugar Barrio Jove de Arriba, 0 S\/N, 33290 Gij\u00f3n, Spain"}]},{"given":"Beatriz","family":"V\u00e1zquez-Belda","sequence":"additional","affiliation":[{"name":"Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Veterinary Medicine, University of Santiago de Compostela, 27002 Lugo, Spain"}]},{"given":"Carlos","family":"Franco","sequence":"additional","affiliation":[{"name":"Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Veterinary Medicine, University of Santiago de Compostela, 27002 Lugo, Spain"}]},{"given":"Alberto","family":"Cepeda","sequence":"additional","affiliation":[{"name":"Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Veterinary Medicine, University of Santiago de Compostela, 27002 Lugo, Spain"}]}],"member":"1968","published-online":{"date-parts":[[2015,12,24]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"2853","DOI":"10.1098\/rstb.2010.0134","article-title":"Livestock production: Recent trends, future prospects","volume":"365","author":"Thornton","year":"2010","journal-title":"Philos. Trans. R. Soc."},{"key":"ref_2","doi-asserted-by":"crossref","first-page":"399","DOI":"10.1897\/IEAM_2008-002.1","article-title":"A ranking of European veterinary medicines based on environmental risks","volume":"4","author":"Kools","year":"2008","journal-title":"Integr. Environ. Assess. Manag."},{"key":"ref_3","doi-asserted-by":"crossref","first-page":"6543","DOI":"10.1007\/s00216-013-7060-5","article-title":"Wide-scope analysis of veterinary drug and pesticide residues in animal feed by liquid chromatography coupled to quadrupole-time-of-flight mass spectrometry","volume":"405","year":"2013","journal-title":"Anal. Bioanal. Chem."},{"key":"ref_4","doi-asserted-by":"crossref","first-page":"342","DOI":"10.1007\/s00128-004-0590-y","article-title":"Multi-residue analysis of pesticides in animal feed concentrate","volume":"74","author":"Sharma","year":"2005","journal-title":"Bull. Environ. Contam. Toxicol."},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"85","DOI":"10.1365\/s10337-006-0112-7","article-title":"Analysis of nitrofuran residues in animal feed using liquid chromatography and photodiode-array detection","volume":"65","author":"Vinas","year":"2007","journal-title":"Chromatographia"},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"1701","DOI":"10.5740\/jaoacint.11-523","article-title":"Analysis of deoxynivalenol, zearalenone, T-2, and HT-2 toxins in animal feed by LC\/MS\/MS-A critical comparison of immunoaffinity column clean-up with no clean-up","volume":"95","author":"Senyuva","year":"2012","journal-title":"J. AOAC Int."},{"key":"ref_7","first-page":"119","article-title":"Detection of aflatoxins, trichothecenes and zearalenone in food and animal feed by reversed phase HPLC and SPE","volume":"963","author":"Varzakas","year":"2012","journal-title":"I Int. Symp. Mycotoxins Nuts Dried Fruits"},{"key":"ref_8","doi-asserted-by":"crossref","first-page":"1222","DOI":"10.1002\/rcm.4979","article-title":"Determination of aflatoxins in animal feeds by liquid chromatography\/tandem mass spectrometry with isotope","volume":"25","author":"Li","year":"2011","journal-title":"Rapid Commun. Mass Spectrom."},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"2091","DOI":"10.1002\/jssc.200800075","article-title":"Chromatographic analysis of banned antibacterial growth promoters in animal feed","volume":"31","author":"Samanidou","year":"2008","journal-title":"J. Sep. Sci."},{"key":"ref_10","doi-asserted-by":"crossref","first-page":"3027","DOI":"10.1007\/s00216-010-3523-0","article-title":"Quantitative analysis of penicillins in porcine tissues, milk and animal feed using derivatisation with piperidine and stable isotope dilution liquid chromatography tandem mass spectrometry","volume":"396","author":"Mulder","year":"2010","journal-title":"Anal. Bioanal. Chem."},{"key":"ref_11","doi-asserted-by":"crossref","first-page":"241","DOI":"10.1079\/BJN19730030","article-title":"Feeding trials with lysine-fortified and threonine-fortified rice","volume":"30","author":"Pereira","year":"1973","journal-title":"Br. J. Nutr."},{"key":"ref_12","doi-asserted-by":"crossref","first-page":"145","DOI":"10.1016\/j.aca.2004.08.012","article-title":"Determination of tetracycline residues in shrimp and whole milk using liquid chromatography with ultraviolet detection and residue confirmation by mass spectrometry","volume":"529","author":"Andersen","year":"2005","journal-title":"Anal. Chim. Acta"},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"328","DOI":"10.1016\/j.foodchem.2013.11.008","article-title":"Ultrasound-assisted dispersive extraction for the high pressure liquid chromatographic determination of Tetracyclines residues in milk with diode array detection","volume":"150","author":"Karageorgou","year":"2014","journal-title":"Food Chem."},{"key":"ref_14","doi-asserted-by":"crossref","first-page":"374","DOI":"10.1016\/j.talanta.2014.04.049","article-title":"A simple, fast and cheap non-SPE screening method for antibacterial residue analysis in milk and liver using liquid chromatography-tandem mass spectrometry","volume":"129","author":"Martins","year":"2014","journal-title":"Talanta"},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"42","DOI":"10.1016\/j.jchromb.2008.04.027","article-title":"Analysis of tetracycline residues in royal jelly by liquid chromatography-tandem mass spectrometry","volume":"868","author":"Xu","year":"2008","journal-title":"J. Chromatogr. B"},{"key":"ref_16","unstructured":"AOAC Official Methods (2008). Oxytetracycline\/oxytetracycline hydrochloride in animal feed, fish feed and animal remedies. Off. Methods Anal. AOAC Int., 18, 82\u201387."},{"key":"ref_17","unstructured":"(2002). Comission Decission 2002\/657\/EC. Commission Decision of 12 August 2002 implementing Council Directive 96\/23\/EC concerning the performance of analytical methods and the interpretation of results. Off. J. Eur. Union, 221, 8\u201336."},{"key":"ref_18","doi-asserted-by":"crossref","first-page":"143","DOI":"10.1016\/S0003-2670(01)01590-2","article-title":"Quantitative analysis for oxytetracycline in medicated premixes and feeds by second-derivative synchronous spectrofluorimetry","volume":"455","year":"2002","journal-title":"Anal. Chim. Acta"},{"key":"ref_19","doi-asserted-by":"crossref","first-page":"54","DOI":"10.1016\/j.aca.2008.01.026","article-title":"Determination of oxytetracycline, tetracycline and chloramphenicol antibiotics in animal feeds using subcritical water extraction and high performance liquid chromatography","volume":"619","author":"Wang","year":"2008","journal-title":"Anal. Chim. Acta"},{"key":"ref_20","doi-asserted-by":"crossref","first-page":"167","DOI":"10.1016\/0378-4347(94)00434-7","article-title":"Determination of oxytetracycline in the live fish feed Artemia using high-performance liquid chromatography with ultraviolet detection","volume":"663","author":"Touraki","year":"1995","journal-title":"J. Chromatogr. B"},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"60","DOI":"10.1016\/j.chroma.2013.03.078","article-title":"Analysis of antimicrobial agents in pig feed by liquid chromatography coupled to orbitrap mass spectrometry","volume":"1293","author":"Kaklamanos","year":"2013","journal-title":"J. Chromatogr. A"},{"key":"ref_22","doi-asserted-by":"crossref","first-page":"6394","DOI":"10.1016\/j.chroma.2010.08.024","article-title":"Development of a multi-class method for the quantification of veterinary drug residues in feeding stuffs by liquid chromatography-tandem mass spectrometry","volume":"1217","author":"Boscher","year":"2010","journal-title":"J. Chromatogr. A"},{"key":"ref_23","doi-asserted-by":"crossref","first-page":"58","DOI":"10.1016\/j.meatsci.2014.04.003","article-title":"Multi-residue and multi-class method for the determination of antibiotics in bovine muscle by ultra-high-performance liquid chromatography tandem mass spectrometry","volume":"98","author":"Freitas","year":"2014","journal-title":"Meat Sci."},{"key":"ref_24","doi-asserted-by":"crossref","first-page":"495","DOI":"10.1016\/j.foodcont.2014.05.042","article-title":"Monitoring the presence of residues of Tetracyclines in baby food samples by HPLC-MS\/MS","volume":"46","author":"Nebot","year":"2014","journal-title":"Food Control"},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"3424","DOI":"10.1016\/j.scitotenv.2010.03.049","article-title":"Simultaneous determination of four classes of antibiotics in sediments of the Pearl Rivers using RRLC\u2013MS\/MS","volume":"408","author":"Yang","year":"2010","journal-title":"Sci. Total Environ."}],"container-title":["Antibiotics"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/2079-6382\/5\/1\/1\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,11]],"date-time":"2025-10-11T20:54:44Z","timestamp":1760216084000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/2079-6382\/5\/1\/1"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2015,12,24]]},"references-count":25,"journal-issue":{"issue":"1","published-online":{"date-parts":[[2016,3]]}},"alternative-id":["antibiotics5010001"],"URL":"https:\/\/doi.org\/10.3390\/antibiotics5010001","relation":{},"ISSN":["2079-6382"],"issn-type":[{"value":"2079-6382","type":"electronic"}],"subject":[],"published":{"date-parts":[[2015,12,24]]}}}