Determination of Tetracycline Antibiotic Residue Levels in Goldfish (Cyprinus carpio) Using High Performance Liquid Chromatography (HPLC)

Agung Abadi Kiswandono, Anisa Rahmawati, Yanesta Oxvyena, Purna Pirdaus, Sonny Widiarto, Sutopo Hadi, Rinawati Rinawati

Abstract

The method for determining residual levels of tetracycline antibiotics in goldfish (Cyprinus carpio) was validated using High Performance Liquid Chromatography (HPLC). The HPLC method has advantages, including high accuracy, efficiency, ease of operation, and high selectivity and sensitivity. This research aims to develop a method for determining tetracycline residues and tetracycline levels in goldfish meat obtained from eight markets in Bandar Lampung City. The analytical method carried out was optimized for the composition and flow rate of the mobile phase. Optimization results show a composition of acetonitrile:water = 35:65 and a flow rate of 0.5 mL/minute. The method validation parameters carried out are linearity, precision, accuracy, selectivity, Limit of Detection (LoD), and Limit of Quantitation (LoQ). The linearity results obtained from this research were R2 = 0.9980. This method has repeatability precision with a Relative Standard Deviation (%RSD) value of 1.35%, and reproducibility precision with %RSD values of 0.96% and 1.14%, respectively. The %recovery method value is 101.05%. The LoD and LoQ values for this method are 0.27 and 0.90 ppm. Measurement of tetracycline antibiotic residue levels in carp samples from 8 market locations in Bandar Lampung showed values of 21.77 – 38.58 ppm, with uncertainties of ±0.87 – ±1.42. The method validation results show that the method can be used for routine analysis of tetracycline antibiotic levels in the laboratory.

Keywords

fish; rate HPLC; tetracycline; validation.

References

Abera, B.D., Ortiz-Gómez, I., Shkodra, B., J. Romero, F., Cantarella, G., Petti, L., Salinas-Castillo, A., Lugli, P., and Rivadeneyra, A., 2021. Laser-Induced Graphene Electrodes Modified with a Molecularly Imprinted Polymer for Detection of Tetracycline in Milk and Meat. Sensors, 22, 269. https://doi.org/10.3390/s22010269.

Alarape, S.A., and Adeyemo, O.K., 2017. Tetracycline Residue in Fresh and Processed Clarias Gariepinus from Selected Fish Farms and Markets in Ibadan, Nigeria. Tropical Veterinarian, 35.

Alhaji, N.B., Maikai, B.-V., and Kwaga, J.K.P., 2021. Antimicrobial Use, Residue and Resistance Dissemination in Freshwater Fish Farms of North-Central Nigeria: One Health Implications. Food Control, 130, 108238. https://doi.org/10.1016/j.foodcont.2021.108238.

Barani, A., and Fallah, A.A., 2015. Occurrence of Tetracyclines, Sulfonamides, Fluoroquinolones and Florfenicol in Farmed Rainbow Trout in Iran. Food and Agricultural Immunology, 26, 420–429. https://doi.org/10.1080/09540105.2014.950199.

Caniça, M., Manageiro, V., Abriouel, H., Moran-Gilad, J., and Franz, C.M.A.P., 2019. Antibiotic Resistance in Foodborne Bacteria. Trends in Food Science & Technology, 84, 41–44. https://doi.org/10.1016/j.tifs.2018.08.001.

Codex Alimentarius Commission International Food Standards, 2017. Maximum Residue Limits for Residues of Veterinary Drugs in Foods. Update as at the 40th Session of the Codex Alimentarius Commission.

Cui, C., Han, Q., Jiang, L., Ma, L., Jin, L., Zhang, D., Lin, K., and Zhang, T., 2018. Occurrence, Distribution, and Seasonal Variation of Antibiotics in an Artificial Water Source Reservoir in the Yangtze River Delta, East China. Environmental Science and Pollution Research, 25, 19393–19402. https://doi.org/10.1007/s11356-018-2124-x.

Daghrir, R., and Drogui, P., 2013. Tetracycline Antibiotics in the Environment: A Review. Environmental Chemistry Letters, 11, 209–227. https://doi.org/10.1007/s10311-013-0404-8.

Dagron, S., 2014. Die International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH), in: Handbuch Ethik Und Recht Der Forschung Am Menschen. Springer Berlin Heidelberg, Berlin, Heidelberg, pp. 541–545. https://doi.org/10.1007/978-3-642-35099-3_86.

Eurachem, G., 2014. The Fitness for Purpose of Analytical Methods, A Laboratory Guide to Method Validation and Related Topics. London, Laboratory of the Government Chemists.

Farmakope Indonesia Edisi IV, 1995. Departemen Kesehatan Republik Indonesia.

Guidelines for Standard Method Performance Requirements, Appendix F, 2012. Association of Official Analytical Chemists (AOAC).

He, S., Wang, Q., Li, S., Ran, C., Guo, X., Zhang, Z., and Zhou, Z., 2017. Antibiotic Growth Promoter Olaquindox Increases Pathogen Susceptibility in Fish by Inducing Gut Microbiota Dysbiosis. Science China Life Sciences, 60, 1260–1270. https://doi.org/10.1007/s11427-016-9072-6.

Laboratory Quality Assurance Division, 2007. Qualitative Identification of Tetracyclines. USA, United States Department of Agriculture Food Safety and Inspection Service.

Lastauskienė, E., Valskys, V., Stankevičiūtė, J., Kalcienė, V., Gėgžna, V., Kavoliūnas, J., Ružauskas, M., and Armalytė, J., 2021. The Impact of Intensive Fish Farming on Pond Sediment Microbiome and Antibiotic Resistance Gene Composition. Frontiers in Veterinary Science, 8. https://doi.org/10.3389/fvets.2021.673756.

Li, W., Shi, C., Yu, Y., Ruan, Y., Kong, D., Lv, X., Xu, P., Awasthi, M.K., and Dong, M., 2021. Interrelationships between Tetracyclines and Nitrogen Cycling Processes Mediated by Microorganisms: A Review. Bioresource Technology, 319, 124036. https://doi.org/10.1016/j.biortech.2020.124036.

Liu, X., Steele, J.C., and Meng, X.-Z., 2017. Usage, Residue, and Human Health Risk of Antibiotics in Chinese Aquaculture: A Review. Environmental Pollution, 223, 161–169. https://doi.org/10.1016/j.envpol.2017.01.003.

Morshdy, A.E.M.A., Hussein, M.A.M., Mohamed, M.A.A., Hamed, E., El-Murr, A.E., and Darwish, W.S., 2022. Tetracycline Residues in Tilapia and Catfish Tissue and the Effect of Different Cooking Methods on Oxytetracycline and Doxycycline Residues. Journal of Consumer Protection and Food Safety, 17, 387–393. https://doi.org/10.1007/s00003-022-01389-7.

Önal, A., 2011. Overview on Liquid Chromatographic Analysis of Tetracycline Residues in Food Matrices. Food Chemistry, 127, 197–203. https://doi.org/10.1016/j.foodchem.2011.01.002.

Orlando, E.A., and Simionato, A.V.C., 2013. Extraction of Tetracyclinic Antibiotic Residues from Fish Filet: Comparison and Optimization of Different Procedures Using Liquid Chromatography with Fluorescence Detection. Journal of Chromatography A, 1307, 111–118. https://doi.org/10.1016/j.chroma.2013.07.084.

Postigo, C., and Richardson, S.D., 2014. Transformation of Pharmaceuticals during Oxidation/Disinfection Processes in Drinking Water Treatment. Journal of Hazardous Materials, 279, 461–475. https://doi.org/10.1016/j.jhazmat.2014.07.029.

Preena, P.G., Dharmaratnam, A., Raj, N.S., Kumar, T.V.A., Raja, S.A., and Swaminathan, T.R., 2019. Antibiotic Susceptibility Pattern of Bacteria Isolated from Freshwater Ornamental Fish, Guppy Showing Bacterial Disease. Biologia, 74, 1055–1062. https://doi.org/10.2478/s11756-019-00261-8.

Preena, P.G., Dharmaratnam, A., Raj, N.S., Raja, S.A., Nair, R.R., and Swaminathan, T.R., 2021. Antibiotic-Resistant Enterobacteriaceae from Diseased Freshwater Goldfish. Archives of Microbiology, 203, 219–231. https://doi.org/10.1007/s00203-020-02021-8.

Rama, C., Rao, M., Cyril, L., Kumar, A., and Sekharan, C.B., 2015. Quantitative Analysis of Oxytetracycline Residues in Honey by High Performance Liquid Chromatography. International Research Journal of Biological Sciences, 4.

Saleh, H., Elhenawee, M., Hussien, E.M., Ahmed, N., and Ibrahim, A.E., 2021. Validation of HPLC-UV Multi-Residue Method for the Simultaneous Determination of Tetracycline, Oxytetracycline, Spiramycin and Neospiramycin in Raw Milk. Food Analytical Methods, 14. https://doi.org/10.1007/s12161-020-01838-9.

Shalaby, A.R., Salama, N.A., Abou-Raya, S.H., Emam, W.H., and Mehaya, F.M., 2011. Validation of HPLC Method for Determination of Tetracycline Residues in Chicken Meat and Liver. Food Chemistry, 124, 1660–1666. https://doi.org/10.1016/j.foodchem.2010.07.048.

SNI 01-6366-2000, 2000. Batas Maksimum Cemaran Mikroba dan Batas Maksimum Residu dalam Bahan Makanan Asal Hewan. Badan Standardisasi Nasional.

Urbano, V.R., Maniero, M.G., Pérez-Moya, M., and Guimarães, J.R., 2017. Influence of PH and Ozone Dose on Sulfaquinoxaline Ozonation. Journal of Environmental Management, 195, 224–231. https://doi.org/10.1016/j.jenvman.2016.08.019.

Wang, H., Wang, N., Wang, B., Fang, H., Fu, C., Tang, C., Jiang, F., Zhou, Y., He, G., Zhao, Q., Chen, Y., and Jiang, Q., 2016. Antibiotics Detected in Urines and Adipogenesis in School Children. Environment International, 89–90, 204–211. https://doi.org/10.1016/j.envint.2016.02.005.

Wang, M., and Helbling, D.E., 2016. A Non-Target Approach to Identify Disinfection Byproducts of Structurally Similar Sulfonamide Antibiotics. Water Research, 102, 241–251. https://doi.org/10.1016/j.watres.2016.06.042.

Zhou, M., Yu, S., Hong, B., Li, J., Han, H., and Qie, G., 2021. Antibiotics Control in Aquaculture Requires More than Antibiotic-Free Feeds: A Tilapia Farming Case. Environmental Pollution, 268, 115854. https://doi.org/10.1016/j.envpol.2020.115854.

DOI: https://doi.org/10.20961/alchemy.22.1.90319.%25p

Refbacks

  • There are currently no refbacks.