Multiresidue chromatographic method for the determination of antibiotic residues in honey by high-performance liquid chromatography with DAD detection

Year 2022, , 157 - 161, 30.12.2022

Bouchra Rachid , Ali Jaber , Edmond Cheble

https://doi.org/10.46239/ejbcs.1104606

Abstract

Clandestinely, consumers may be exposed to antibiotic (ATB) residues in honey, which could pose a health concern. For the first time, the simultaneous determination of Florfenicol (FF), Penicillin G (PG), and Tetracycline is described in this paper. The multiresidual method was developed and optimized using high-performance liquid chromatography (HPLC) coupled to a diode array detector (DAD). These ATBs were separated on a C18 analytical column after a cleanup process followed by solid-phase extraction (SPE). For the first time, the chromatographic conditions were perfected. After the method validation process, the method was used to assess ATB residues in four Lebanese honey samples. ATBs were separated in less than 15 min with an isocratic elution using a mixture of 80 % potassium dihydrogen phosphate aqueous solution, and 20 % acetonitrile. The UV detection was performed at 350 nm for TC, 224 nm for FF, and 230 nm for PG. The proposed method was linear (R2 ≥ 0.996) within the concentration ranges of 0.7-17.5 mg.Kg 1 for the three compounds. Both intra- and inter-day precision, expressed as RSD, were ≤15 %. The method was subsequently successfully applied to analyze examined ATB residues in honey samples collected from Lebanese beekeeping. The method described could be a valuable tool to conduct a comprehensive survey of honey samples produced in Lebanon, especially in the lack of serious national oversight.

Keywords

Multiresidue, Antibiotics, HPLC-DAD, Honey, SPE

References

• Abraham, J. (2010). International Conference On Harmonisation Of Technical Requirements For Registration Of Pharmaceuticals For Human Use. In C. Tietje & A. Brouder (Eds.), Handbook of Transnational Economic Governance Regimes (pp. 1041–1053). Brill | Nijhoff. https://doi.org/10.1163/ej.9789004163300.i-1081.897
• Bensakhria, A. (2016, October 28). Chromatographie Liquide Haute Performance (HPLC) » Analytical Toxicology. Analytical Toxicology. https://www.analyticaltoxicology.com/chromatographie-liquide-haute-performance-hplc/
• Bonerba, E., Panseri, S., Arioli, F., Nobile, M., Terio, V., Di Cesare, F., Tantillo, G., & Maria Chiesa, L. (2021). Determination of antibiotic residues in honey in relation to different potential sources and relevance for food inspection. Food Chemistry, 334, 127575. https://doi.org/10.1016/j.foodchem.2020.127575
• Cinquina, A. L., 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. https://doi.org/10.1016/S0021-9673(02)01446-2
• Dawadi, S., Thapa, R., Modi, B., Bhandari, S., Timilsina, A. P., Yadav, R. P., Aryal, B., Gautam, S., Sharma, P., Thapa, B. B., Aryal, N., Aryal, S., Regmi, B. P., & Parajuli, N. (2021). Technological Advancements for the Detection of Antibiotics in Food Products. Processes, 9(9), 1500. https://doi.org/10.3390/pr9091500
• European Commission. (102 C.E.). Commission Regulation (EU) No 37/2010 of 22 December 2009 on pharmacologically active substances and their classification regarding maximum residue limits in foodstuffs of animal origin. 5(470), 1–72.
• European Commission. (2002). Commission Decision of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results. L221/8, 8–36.
• Forsgren, E. (2010). European foulbrood in honey bees. Journal of Invertebrate Pathology, 103, S5–S9. https://doi.org/10.1016/j.jip.2009.06.016
• Gaudin, V. (2016). Caractérisation de la performance et validation des méthodes de dépistage des résidus d’antibiotiques dans les denrées alimentaires. Université Rennes 1.
• Johnson, S., & Jadon, N. (2010). Antibiotic Residues in Honey (pp. 1–48). Centre for Science and Environment. https://cdn.cseindia.org/userfiles/Antiboitics_Honey.pdf
• Kumar, A., Gill, J. P. S., Bedi, J. S., Chhuneja, P. K., & Kumar, A. (2020). Determination of antibiotic residues in Indian honeys and assessment of potential risks to consumers. Journal of Apicultural Research, 59(1), 25–34. https://doi.org/10.1080/00218839.2019.1677000
• Lana, S., & Marwan, M. (2016). Honey: Lebanons Golden Elixir (pp. 1–5). BLOMINVEST BANK. https://blog.blominvestbank.com/wp-content/uploads/2016/11/Honey-Lebanons-Golden-Elixir-2.pdf
• Liang, Y., Denton, M. B., & Bates, R. B. (1998). Stability studies of tetracycline in methanol solution. Journal of Chromatography A, 827(1), 45–55. https://doi.org/10.1016/S0021-9673(98)00755-9
• Lima, C. M. G., Nora, F. M. D., Seraglio, S. K. T., Silva, J. M. da, Marzoque, H. J., Santana, R. F., Verruck, S., & Scussel, V. M. (2020). Antibiotic residues in honey: A public health issue. Research, Society and Development, 9(11), e1739119604–e1739119604. https://doi.org/10.33448/rsd-v9i11.9604
• Majewska, E., Drużyńska, B., & Wołosiak, R. (2019). Determination of the botanical origin of honeybee honeys based on the analysis of their selected physicochemical parameters coupled with chemometric assays. Food Science and Biotechnology, 28(5), 1307–1314. https://doi.org/10.1007/s10068-019-00598-5
• Orso, D., Floriano, L., Ribeiro, L. C., Bandeira, N. M. G., Prestes, O. D., & Zanella, R. (2016). Simultaneous Determination of Multiclass Pesticides and Antibiotics in Honey Samples Based on Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry. Food Analytical Methods, 9(6), 1638–1653. https://doi.org/10.1007/s12161-015-0339-8
• Peris-Vicente, J., Peris-García, E., Albiol-Chiva, J., Durgbanshi, A., Ochoa-Aranda, E., Carda-Broch, S., Bose, D., & Esteve-Romero, J. (2022). Liquid chromatography, a valuable tool in the determination of antibiotics in biological, food and environmental samples. Microchemical Journal, 177, 107309. https://doi.org/10.1016/j.microc.2022.107309
• Prichard, F. E., Prichard, E., & Green, J. (2001). Analytical Measurement Terminology: Handbook of Terms Used in Quality Assurance of Analytical Measurement. Royal Society of Chemistry.
• Serwecińska, L. (2020). Antimicrobials and Antibiotic-Resistant Bacteria: A Risk to the Environment and to Public Health. Water, 12(12), 3313. https://doi.org/10.3390/w12123313
• Shabir, G. A. (2010). Development and Validation of a Reversed-phase HPLC Method for the Determination of Hydroxybenzene in a Cream Formulation. Indian Journal of Pharmaceutical Sciences, 72(3), 307–311. https://doi.org/10.4103/0250-474X.70475
• United Nations Office on Drugs and Crime & Laboratory and Scientific Section. (2009). Guidance for the validation of analytical methodology and calibration of equipment used for testing of illicit drugs in seized materials and biological specimens: A commitment to quality and continuous improvement. United Nations.
• Vidal-Naquet, N. (2012). Les maladies de l’abeille domestique d’élevage, Apis mellifera l. Bulletin de l’Académie Vétérinaire de France, 165(4), 307–316. https://doi.org/10.4267/2042/48811