{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,9,29]],"date-time":"2026-09-29T00:13:51Z","timestamp":1790640831994,"version":"4.1.0"},"reference-count":38,"publisher":"MDPI AG","issue":"9","license":[{"start":{"date-parts":[[2020,5,5]],"date-time":"2020-05-05T00:00:00Z","timestamp":1588636800000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Molecules"],"abstract":"<jats:p>The presence of tetracycline (TC) antibiotics was determined in animal feed that had been previously screened with a microbiological plate test. Feed samples were screened by a microbiological plate test on a pH 6.0 culture medium seeded with Bacillus cereus ATCC 11778 able to pre-reveal the presence of tetracyclines. Subsequently, confirmation and quantification were performed using a validated HPLC method with mass spectrometric detection. In 2013\u20132018, 353 feed samples were analysed to detect antibacterial substances, of which 186 (52.7%) were suspected to contain tetracyclines. Forty-two out of 186 (22.6%) samples analysed by the chromatographic method contained undeclared tetracyclines, which were determined at concentrations from 0.3 to 49 mg kg\u22121. The most frequently identified contaminating tetracyclines were doxycycline and chlortetracycline.<\/jats:p>","DOI":"10.3390\/molecules25092162","type":"journal-article","created":{"date-parts":[[2020,5,7]],"date-time":"2020-05-07T04:46:07Z","timestamp":1588826767000},"page":"2162","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":20,"title":["Contamination of Animal Feed with Undeclared Tetracyclines\u2014Confirmatory Analysis by Liquid Chromatography\u2013Mass Spectrometry after Microbiological Plate Test"],"prefix":"10.3390","volume":"25","author":[{"given":"Monika","family":"Przenios\u0142o-Siwczy\u0144ska","sequence":"first","affiliation":[{"name":"Department of Hygiene of Animal Feedingstuffs, National Veterinary Research Institute, Partyzantow 57 Avenue, 24-100 Pulawy, Poland"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3827-2314","authenticated-orcid":false,"given":"Ewelina","family":"Patyra","sequence":"additional","affiliation":[{"name":"Department of Hygiene of Animal Feedingstuffs, National Veterinary Research Institute, Partyzantow 57 Avenue, 24-100 Pulawy, Poland"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Aleksandra","family":"Grelik","sequence":"additional","affiliation":[{"name":"Department of Hygiene of Animal Feedingstuffs, National Veterinary Research Institute, Partyzantow 57 Avenue, 24-100 Pulawy, Poland"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Maja","family":"Chy\u0142ek-Purcha\u0142a","sequence":"additional","affiliation":[{"name":"Department of Hygiene of Animal Feedingstuffs, National Veterinary Research Institute, Partyzantow 57 Avenue, 24-100 Pulawy, Poland"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Beata","family":"Kozak","sequence":"additional","affiliation":[{"name":"Department of Hygiene of Animal Feedingstuffs, National Veterinary Research Institute, Partyzantow 57 Avenue, 24-100 Pulawy, Poland"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Krzysztof","family":"Kwiatek","sequence":"additional","affiliation":[{"name":"Department of Hygiene of Animal Feedingstuffs, National Veterinary Research Institute, Partyzantow 57 Avenue, 24-100 Pulawy, Poland"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"1968","published-online":{"date-parts":[[2020,5,5]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"305","DOI":"10.1111\/j.1365-2885.1996.tb00054.x","article-title":"Bioavailability of oxytetracycline, tetracycline and chlortetracycline after oral administration to fed and fasted pigs","volume":"19","author":"Nielsen","year":"1996","journal-title":"J. Vet. Pharmacol. Ther."},{"key":"ref_2","unstructured":"Gorbach, S.L., Bartlett, J.G., and Blacklow, N.R. (1998). Tetracyclines. Infectious diseases, The W.B. Saunders Co.. [2nd ed.]."},{"key":"ref_3","doi-asserted-by":"crossref","first-page":"232","DOI":"10.1128\/MMBR.65.2.232-260.2001","article-title":"Tetracyclines Antibiotics: Mode of Action, Applications, Molecular Biology, and Epidemiology of Bacterial Resistance","volume":"65","author":"Chopra","year":"2001","journal-title":"Microbiol. Mol. Biol. Rev."},{"key":"ref_4","doi-asserted-by":"crossref","first-page":"2430","DOI":"10.1002\/jssc.200700057","article-title":"Development and validation of an HPLC confirmatory method for the determination of seven tetracycline antibiotics residues in milk according to the European Union Decision 2002\/657\/EC","volume":"30","author":"Samanidou","year":"2007","journal-title":"J. Sep. Sci."},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"279","DOI":"10.1079\/095442200108729106","article-title":"Antibiotic use in animal feed and its impact on human health","volume":"13","author":"Barton","year":"2000","journal-title":"Nutr. Res. Rev."},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"439","DOI":"10.1016\/j.mib.2003.09.009","article-title":"Antibiotics in animal feed and their role in resistance development","volume":"6","author":"Wegener","year":"2003","journal-title":"Curr. Opin. Microbiol."},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"79","DOI":"10.1177\/003335490712200111","article-title":"Growth Promoting Antibiotics in Food Animal Production: An Economic Analysis","volume":"122","author":"Graham","year":"2007","journal-title":"Public Health Rep."},{"key":"ref_8","unstructured":"Swann, M.M. (1969). Report of the Joint Committee on the Use of Antibiotics in Animal Husbandry and Veterinary Medicine, Her Majesty\u2019s Stationery Office."},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"996","DOI":"10.1126\/science.279.5353.996","article-title":"Medical Consequences of Antibiotics Use in Agriculture","volume":"279","author":"Witte","year":"1998","journal-title":"Science"},{"key":"ref_10","doi-asserted-by":"crossref","first-page":"718","DOI":"10.1128\/CMR.00002-11","article-title":"Food Animals and Antimicrobials: Impacts on Human Health","volume":"24","author":"Marschall","year":"2011","journal-title":"Clin. Microbiol. Rev."},{"key":"ref_11","doi-asserted-by":"crossref","first-page":"2466","DOI":"10.3382\/ps.2007-00249","article-title":"History of the use of antibiotic as growth promoters in european poultry feeds","volume":"86","author":"Castanon","year":"2007","journal-title":"Poultry Science"},{"key":"ref_12","doi-asserted-by":"crossref","first-page":"359","DOI":"10.1007\/s002030050339","article-title":"Tetracyclines: Antibiotic action, uptake, and resistance mechanisms","volume":"165","author":"Schnappinger","year":"1996","journal-title":"Arch. Microbiol."},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"2284","DOI":"10.1093\/jac\/dku106","article-title":"Variations in the sales and sales patterns of veterinary antimicrobial agents in 25 European countries","volume":"69","author":"Grave","year":"2014","journal-title":"J. Antimicrob. Chemother."},{"key":"ref_14","unstructured":"European Medicines Agency (2019). Sales of Veterinary Antimicrobial Agents in 31 European Countries in 2017, European Medicines Agency. Ninht ESVAC Report."},{"key":"ref_15","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 feedingstuffs by liquid chromatography-tandem mass spectrometry","volume":"1217","author":"Boscher","year":"2010","journal-title":"J. Chromatogr. A"},{"key":"ref_16","doi-asserted-by":"crossref","first-page":"527","DOI":"10.1515\/bvip-2015-0079","article-title":"Occurrence of tetracyclines in feedingstuffs\u2013results of a two-year study within the official control of feed","volume":"59","author":"Patyra","year":"2015","journal-title":"Bull. Vet. Inst. Pulawy"},{"key":"ref_17","unstructured":"European Commission (2003). Regulation (EC) No 1831\/2003 of the European Parliament and of the Council of 22 September 2003 on Additives for Use in Animal Nutrition, European Commission. OJ L268."},{"key":"ref_18","unstructured":"European Commission (2019). Regulation (EU) No 2019\/4 of the European Parliament and of the Council of on the manufacture, placing on the market and use of medicated feed, amending Regulation (EC) No 183\/2005 of the European Parliament and of the Council and repealing Council Directive 90\/167\/EEC, European Commission. OJ L4."},{"key":"ref_19","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_20","doi-asserted-by":"crossref","first-page":"1100","DOI":"10.1080\/19440049.2013.794308","article-title":"Carry-over of veterinary drugs from medicated to non-medicated feeds in commercial feed manufacturing plants","volume":"30","author":"Stolker","year":"2013","journal-title":"Food Addit. Contam. Part A"},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"101","DOI":"10.1016\/S0924-8579(98)00093-4","article-title":"EU conference \u2018The Microbial Threat\u201d","volume":"11","author":"Mevius","year":"1999","journal-title":"Int. J. Antimicrob. Ag"},{"key":"ref_22","doi-asserted-by":"crossref","unstructured":"Barug, D., de Jong, J., Kies, A.K., and Verstegen, M.W.A. (2006). Towards a control strategy for banned antibiotics and growth promoters in feed: The SIMBAG-FEED project. Antimicrobial Growth Promoters. Where do we go from here?, Wageningen Academic Publishers. [1st ed.].","DOI":"10.3920\/978-90-8686-570-3"},{"key":"ref_23","doi-asserted-by":"crossref","first-page":"2737","DOI":"10.1039\/a804909b","article-title":"Detection of residues of tetracycline antibiotics in pork and chicken meat: Correlation between results of screening and confirmatory tests","volume":"123","author":"Okerman","year":"1998","journal-title":"Analyst"},{"key":"ref_24","doi-asserted-by":"crossref","first-page":"528","DOI":"10.1080\/0265203031000098696","article-title":"Residues of \u03b2-lactams antibiotics in bovine milk: Confirmatory analysis by liquid chromatography tandem mass spectrometry after microbial assay screening","volume":"20","author":"Ghidini","year":"2003","journal-title":"Food Addit. Contam."},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"1042","DOI":"10.1016\/j.trac.2011.02.012","article-title":"Analysis of antimicrobial agents in animal feed","volume":"30","author":"Borras","year":"2011","journal-title":"Trends Anal. Chem."},{"key":"ref_26","doi-asserted-by":"crossref","unstructured":"Chico, J., van Holthoon, F., and Zuidema, T. (2012). Ion Suppression Study for Tetracyclines in Feed. Chromatogr. Res. Int., 9.","DOI":"10.1155\/2012\/135854"},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"3","DOI":"10.1016\/S0003-2670(02)00751-1","article-title":"Contamination of animal feedingstuffs as a cause of residues in food: A review of regulatory aspects, incidence and control","volume":"473","author":"McEvoy","year":"2002","journal-title":"Anal. Chim. Acta"},{"key":"ref_28","doi-asserted-by":"crossref","first-page":"1195","DOI":"10.1007\/s00216-010-4005-0","article-title":"Determination of antibacterials in animal feed by pressurized liquid extraction followed by online purification and liquid chromatography-electrospray tandem mass spectrometry","volume":"398","author":"Kantiani","year":"2010","journal-title":"Anal. Bioanal. Chem."},{"key":"ref_29","first-page":"11","article-title":"Microbiological screening method for detection of aminoglycosides, \u03b2-lactams, macrolides, tetracyclines and quinolones in meat samples","volume":"44","year":"2007","journal-title":"Slov. Vet. Res."},{"key":"ref_30","doi-asserted-by":"crossref","first-page":"162","DOI":"10.1080\/02652039809374626","article-title":"Contamination of animal feedingstuffs with undeclared antimicrobial additives","volume":"15","author":"Lynas","year":"1998","journal-title":"Food Addit. Contamin."},{"key":"ref_31","doi-asserted-by":"crossref","first-page":"1","DOI":"10.1111\/1574-6941.12093","article-title":"Impact of subtherapeutic administration of tylosin and chlortetracycline on antimicrobial resistance in farrow-to-finish swine","volume":"85","author":"Holman","year":"2013","journal-title":"FEMS Microbiol. Ecol."},{"key":"ref_32","doi-asserted-by":"crossref","first-page":"860","DOI":"10.1080\/19440049.2011.569574","article-title":"Doxycycline and sulfadimethoxine transfer from cross-contaminated feed to chicken tissues","volume":"28","author":"Segato","year":"2011","journal-title":"Food Addit. Contamin."},{"key":"ref_33","unstructured":"World Health Organization (2019). Critically Important Antimicrobials for Human Medicine, World Health Organization. 6th revision."},{"key":"ref_34","doi-asserted-by":"crossref","first-page":"1","DOI":"10.3389\/fmicb.2013.00221","article-title":"Antimicrobial resistance in commensal Escherichia coli isolated from animals at slaughter","volume":"4","author":"Wasyl","year":"2013","journal-title":"Front. Microbiol."},{"key":"ref_35","first-page":"599","article-title":"Evaluation of multi\u2013plate microbial assay for the screening of antibacterial substances in animal feedingstuffs","volume":"51","author":"Kwiatek","year":"2007","journal-title":"Bull. Vet. Inst. Pulawy"},{"key":"ref_36","doi-asserted-by":"crossref","first-page":"1553","DOI":"10.1080\/19440049.2017.1364430","article-title":"Development and validation of multi-residue analysis of tetracycline antibiotics in feed by high performance liquid chromatography coupled with mass spectrometry","volume":"34","author":"Patyra","year":"2017","journal-title":"Food Addit. Contam. A"},{"key":"ref_37","doi-asserted-by":"crossref","first-page":"477","DOI":"10.1016\/0278-6915(91)90095-O","article-title":"Risk assessment of antibiotic residues of beta-lactams and macrolides in food products with regard to their immunoallergic potential","volume":"29","author":"Dewdney","year":"1991","journal-title":"Food Chem. Toxicol."},{"key":"ref_38","doi-asserted-by":"crossref","first-page":"2","DOI":"10.1080\/01652176.2001.9695068","article-title":"Human health hazards associated with the administration of antimicrobials to slaughter animals. Part I. An assessment of the risks of residues of tetracyclines in pork","volume":"23","author":"Berends","year":"2001","journal-title":"Vet. Q."}],"container-title":["Molecules"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/1420-3049\/25\/9\/2162\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,13]],"date-time":"2025-10-13T13:52:57Z","timestamp":1760363577000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/1420-3049\/25\/9\/2162"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2020,5,5]]},"references-count":38,"journal-issue":{"issue":"9","published-online":{"date-parts":[[2020,5]]}},"alternative-id":["molecules25092162"],"URL":"https:\/\/doi.org\/10.3390\/molecules25092162","relation":{},"ISSN":["1420-3049"],"issn-type":[{"value":"1420-3049","type":"electronic"}],"subject":[],"published":{"date-parts":[[2020,5,5]]}}}