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Journal of Apicultural Science

The Journal of Research Institute of Horticulture and Apicultural Research Association

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2299-4831
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Oxytetracycline Residues in Honey Analyzed by Liquid Chromatography with UV Detection

Anna Gajda
  • Corresponding author
  • Department of Pharmacology and Toxicology, National Veterinary Research Institute, Partyzantów 57, 24-100 Pulawy, Poland
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/ Andrzej Posyniak
  • Department of Pharmacology and Toxicology, National Veterinary Research Institute, Partyzantów 57, 24-100 Pulawy, Poland
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/ Andrzej Bober
  • Department of Honey Bee Diseases, National Veterinary Research Institute, Partyzantów 57, 24-100 Pulawy, Poland
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/ Tomasz Błądek
  • Department of Pharmacology and Toxicology, National Veterinary Research Institute, Partyzantów 57, 24-100 Pulawy, Poland
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/ Jan Żmudzki
  • Department of Pharmacology and Toxicology, National Veterinary Research Institute, Partyzantów 57, 24-100 Pulawy, Poland
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Published Online: 2013-06-05 | DOI: https://doi.org/10.2478/jas-2013-0003

Summary

A liquid chromatography method with UV detection for determination of oxytetracycline (OTC) in honey has been developed. The samples were extracted with the solution of oxalic acid. The clean-up procedure was performed by solid phase extraction (SPE) using polymeric Strata X and carboxylic acid cartridges. Chromatographic separation was carried out on the Luna C8 analytical column with mobile phase consisting of acetonitrile-0.02 M oxalic acid. The method has been successfully validated according to the requirements of the European Decision 2002/657/EC and this method is used in routine control of oxytetracycline in honey samples. The limit of detection (LOD) and limit of quantification (LOQ) of the presented method were 10 and 12.5 μg/kg, respectively. The developed method has also been verified in quantitative determination of oxytetracycline residues in honey after experimental treatment with this product in bee colonies.

Streszczenie

Opracowano metodę chromatografii cieczowej z detektorem UV do oznaczania oksytetracykliny (OTC) w miodzie. Do ekstrakcji próbek wykorzystano roztwór kwasu szczawiowego. Do oczyszczania zastosowano zestaw ekstrakcji do fazy stałej (SPE) z użyciem kolumienek polimerycznych Strata X oraz kolumienek karboksylowych. Rozdziału chromatograficznego dokonano przy użyciu kolumny analitycznej Luna C8 z faza ruchomą składającą się z acetonitrylu i 0.02 M roztworu kwasu szczawiowego. Metoda została zwalidowana zgodnie z wymogami Decyzji Komisji Europejskiej 2002/657/EC i jest stosowana w rutynowych badaniach kontrolnych oksytetracykliny w próbkach miodu. Opracowana metoda została zweryfikowana w ilościowym oznaczaniu pozostałości oksytetracykliny w miodzie po eksperymentalnym podaniu pszczołom tego antybiotyku. Celem przeprowadzonego doświadczenia było określenie, jak długo oksytetracyklina może pozostawać w miodzie. Badano także stabilność oksytetracykliny w warunkach laboratoryjnych. Wyniki badania stabilności wskazują, że oksytetracyklina w miodzie przechowywanym w warunkach laboratoryjnych ulega powolnemu zmniejszaniu. W pobranych do badań próbkach miodu stwierdzono zawartość OTC w stężeniach od 17 300 μg/kg do 34 000 μg/kg. Przeprowadzone badania wskazują, że OTC w znacznych ilościach przedostaje się do miodu po jej zastosowaniu u pszczół. Po 12 miesiącach od podania antybiotyku pszczołom, stężenie w miodzie było poniżej wyznaczonej granicy wykrywalności metody (10 μg/kg).

Keywords: oxytetracycline; honey; residues; validation; depletion; HPLC-UV method

Słowa kluczowe: oksytetracyklina; miód; pozostałości; walidacja; zanikanie; metoda HPLC-UV

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About the article

Published Online: 2013-06-05

Published in Print: 2013-06-01


Citation Information: Journal of Apicultural Science, ISSN (Print) 2299-4831, DOI: https://doi.org/10.2478/jas-2013-0003.

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