Detection and Quantification of Oxytetracycline Residues in Raw Semnan Milk Using High-Performance Liquid Chromatography (HPLC) Method

Document Type : Original Article

Authors

1 Faculty of Veterinary Medicine, Semnan, Semnan, Iran

2 Department of Basic Sciences, Faculty of Veterinary Medicine, Semnan University, Semnan, Iran

3 Department of Food Hygiene, Faculty of Veterinary Medicine, Semnan University, Semnan, Iran

4 , Department of Comparative Biosciences, Faculty of Veterinary Medicine, University of Tehran, Tehran, Iran

10.22075/jvlr.2025.38791.1183

Abstract

Tetracyclines are a widely used, broad-spectrum class of antibiotics prescribed to manage mastitis and various diseases in dairy herds.  The improper and excessive use of antibiotics, along with failure to observe withdrawal periods, has led to the presence of drug residues in food products of animal origin. The present study aimed to determine the level of oxytetracycline in raw milk consumed in the city of Semnan. This cross-sectional study was conducted during the autumn. Thirty-six samples were collected from a milk platform in the city of Semnan. The samples were then analyzed for oxytetracycline residues using High-Performance Liquid Chromatography (HPLC). The concentration of oxytetracycline isolated in all samples was less than the Maximum Residue Limit (MRL) of 0.1 µg/mL, with the exception of one sample that was above the limit. Given the presence of drug residues in milk found in this study and others, further investigations into the health of products from treated animals for human consumption should be a priority. The prudent use of antimicrobial drugs and adherence to their withdrawal periods can prevent the adverse effects and harm associated with them.

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Aalipour, F., Mirlohi, M., Jalali, M., & Azadbakht, L. (2015). Dietary exposure to tetracycline residues through milk consumption in Iran. Journal of Environmental Health Science and Engineering, 13(1), 80.
Abbasi, M. M., Babaei, H., & Ansarin, M. (2011). Simultaneous determination of tetracyclines residues in bovine milk samples by solid phase extraction and HPLC-FL method. Advanced pharmaceutical bulletin, 1(1), 34.
Al Zuheir, I. M. (2012). Detection of β-lactams and tetracyclines antimicrobial residues in raw dairy milk for human consumption in Palestine. Walailak Journal of Science and Technology (WJST), 9(3), 277-279.
Boatto, G., Pau, A., Palomba, M., Arenare, L., & Cerri, R. (1999). Monitoring of oxytetracycline in ovine milk by high-performance liquid chromatography. Journal of pharmaceutical and biomedical analysis, 20(1), 321-326.
Cinquina, A., Longo, F., Anastasi, G., Giannetti, L., & Cozzani, R. (2003). Validation of a high-performance liquid chromatography method for the determination of oxytetracycline, tetracycline, chlortetracycline and doxycycline in bovine milk and muscle. Journal of Chromatography A, 987(1), 227-233.
Dabbagh Moghaddam, A., Tayebi, L., Falahatpisheh, H., Mahmoudian, M., Kowsari, N., Akbarein, H., & Sabzikar, A. (2014). Evaluation of the tetracycline residues in pasteurized milks distributed in Tehran by HPLC method. J Army Univ Med Sci, 11(4), 318-323.
Dasenaki, M. E., & Thomaidis, N. S. (2010). Multi-residue determination of seventeen sulfonamides and five tetracyclines in fish tissue using a multi-stage LC–ESI–MS/MS approach based on advanced mass spectrometric techniques. Analytica chimica acta, 672(1), 93-102.
de Faria, H. D., Rosa, M. A., Silveira, A. T., & Figueiredo, E. C. (2017). Direct extraction of tetracyclines from bovine milk using restricted access carbon nanotubes in a column switching liquid chromatography system. Food Chemistry, 225, 98-106.
Elizabeta, D. S., Zehra, H. M., Biljana, S. D., Pavle, S., & Risto, U. (2011). Screening of veterinary drug residues in milk from individual farms in Macedonia. Mac. Vet. Rev, 34(1), 5-13.
Gaurav, A., Gill, J. P. S., Aulakh, R. S., & Bedi, J. S. (2014). ELISA based monitoring and analysis of tetracycline residues in cattle milk in various districts of Punjab. Veterinary World, 7(1), 26-29.
Kaale, E., Chambuso, M., & Kitwala, J. (2008). Analysis of residual oxytetracycline in fresh milk using polymer reversed-phase column. Food chemistry, 107(3), 1289-1293.
Kaya, S. E., & Filazi, A. (2010). Determination of antibiotic residues in milk samples. Kafkas Univ Vet Fak Derg, 16(Suppl-A), S31-S35.
Kimera, Z. I., Mdegela, R. H., Mhaiki, C. J. N., Karimuribo, E. D., Mabiki, F., Nonga, H. E., et al. (2015). Determination of oxytetracycline residues in cattle meat marketed in the Kilosa district, Tanzania. Onderstepoort Journal of Veterinary Research, 82(1), 01-05.
Mamani, M. C. V., Reyes, F. G. R., & Rath, S. (2009). Multiresidue determination of tetracyclines, sulphonamides and chloramphenicol in bovine milk using HPLC-DAD. Food Chemistry, 117(3), 545-552.
Masawat, P., & Slater, J. M. (2007). The determination of tetracycline residues in food using a disposable screen-printed gold electrode (SPGE). Sensors and Actuators B Chemical, 124(1), 127-132.
Nebot, C., Guarddon, M., Seco, F., Iglesias, A., Miranda, J. M., Franco, C. M., et al. (2014). Monitoring the presence of residues of tetracyclines in baby food samples by HPLC-MS/MS. Food Control, 46, 495-501.
Pena, A., Lino, C. M., Alonso, R., & Barcelo, D. (2007). Determination of tetracycline antibiotic residues in edible swine tissues by liquid chromatography with spectrofluorometric detection and confirmation by mass spectrometry. J. Agric. Food Chem, 55, 4973-4979.
Rassouli, A., Abdolmaleki, Z., Bokaee, S., Kamkar, A., & Shams, G. R. (2010). A cross-sectional study on oxytetracycline and tetracycline residues in pasteurized milk supplied in tehran by an HPLC method. Iranian Journal of Veterinary Medicine, 4(1).
Saleh, S. M. K., Mussaed, A. M., & Al-Hariri, F. M. (2016). Determination of Tetracycline and Oxytetracycline Residues in Honey by High Performance Liquid Chromatography. Journal of Agricultural Science and Technology B, 6, 135-139.
Shalaby, A. R., Salama, N. A., Abou-Raya, S. H., Emam, W. H., & Mehaya, F. M. (2011). Validation of HPLC method for determination of tetracycline residues in chicken meat and liver. Food Chemistry, 124(4), 1660-1666.