ABSTRACT:
Milk is considered an essential nutritional source that cannot be dispensed with; therefore, it is crucial to pay special attention to monitoring it, particularly regarding drug residues. This is a new UV spectrophotometric method that is simple, precise, fast, and economical for monitoring the antibiotic Enrofloxacin in milk based on the second-order derivative. Chloroform was used as an extraction solvent, and the drug was determined at a wavelength of 289 nm after centrifugation at 5000 RPM, where milk showed no absorption at this wavelength, unlike the drug. The linearity range was examined and determined to be 0.5–8 µg/mL. The correlation coefficient (R2) was 0.9995. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.03 µg/mL and 0.09 µg/mL respectively. The method shows acceptable linearity, recoveries, accuracy, and precision with percentage relative standard deviation (RSD%) less than 2%. The newly proposed method was validated in accordance with ICH and VICH requirements, and its application on the milk samples was executed.
Cite this article:
Nazira Sarkis, Mustafa Sawass. New Derivative UV Spectroscopic Method for Determination of Enrofloxacin in Milk. Research Journal of Pharmacy and Technology.2025;18(2):699-5. doi: 10.52711/0974-360X.2025.00103
Cite(Electronic):
Nazira Sarkis, Mustafa Sawass. New Derivative UV Spectroscopic Method for Determination of Enrofloxacin in Milk. Research Journal of Pharmacy and Technology.2025;18(2):699-5. doi: 10.52711/0974-360X.2025.00103 Available on: https://rjptonline.org/AbstractView.aspx?PID=2025-18-2-35
6. REFERENCES:
1. Lambrini K, Aikaterini F, Konstantinos K, Christos I, Ioanna PV, Areti T. Milk nutritional composition and its role in human health. Journal of Pharmacy and Pharmacology. 2020; 9(1). Available from: http://dx.doi.org/10.17265/2328-2150/2021.01.002
2. Pereira PC. Milk nutritional composition and its role in human health. Nutrition. 2014; 30(6): 619–27. Available from: http://dx.doi.org/10.1016/j.nut.2013.10.011
3. Rashmi K, Gupta M, Tarapdar S, Duggal M, Tyagi S, Kaur H, et al. Influence of dietary molecules on human health: Whey proteins. Research Journal of Pharmacy and Technology. 2022; 1910–4. Available from: http://dx.doi.org/10.52711/0974-360x.2022.00318
4. Khan MY, Roy M, Saroj BK, Dubey S, Sharma VK. A Review-Benefits of Panchgavya therapy (Cowpathy) for health of humans. Asian Journal of Research in Pharmaceutical Science. 2015; 5(2): 115. Available from: http://dx.doi.org/10.5958/2231-5659.2015.00019.3
5. Sachi S, Ferdous J, Sikder MH, Azizul Karim Hussani SM. Antibiotic residues in milk: Past, present, and future. Journal of Advanced Veterinary and Animal Research. 2019; 6(3): 315–32. Available from: http://dx.doi.org/10.5455/javar.2019.f350
6. Madhuri D, Divya K, Durgaharish V, Dhanunjayam M, Kumar KS. Screening of Adulterants in milk samples of Amaravathi region in Andhra Pradesh. Research Journal of Pharmacy and Technology. 2015;8(12):1633. Available from: http://dx.doi.org/10.5958/0974-360x.2015.00293.0
7. Avula V, Sundar S, Rekha S, Kalpana. Analytical methods to detect the Adulterants in Milk - An Overview. Asian Journal of Research in Pharmaceutical Science. 2022;272–6. Available from: http://dx.doi.org/10.52711/2231-5659.2022.00046
8. Jeena S, Venkateswaramurthy N, Sambathkumar R. Antibiotic residues in milk products: Impacts on human health. Research Journal of Pharmacology and Pharmacodynamics. 2020; 12(1): 15. Available from: http://dx.doi.org/10.5958/2321-5836.2020.00004.x
9. Virto M, Santamarina-García G, Amores G, Hernández I. Antibiotics in dairy production: Where is the problem? Dairy. 2022; 3(3): 541–564. Available from: http://dx.doi.org/10.3390/dairy3030039
10. Al- Kindi S, Yaqoob ALBalushi II, Abdulalim Elshaar AY, Al Kharusi A, Al Maimani R, Ahuja A. Determination of Tetracycline residues in red meat available in Oman. Research Journal of Pharmacy and Technology. 2023; 2182–6. Available from: http://dx.doi.org/10.52711/0974-360x.2023.00358
11. Tentu. Nageswara Rao, D. Sreenivasulu, E.G. Sreenivasula Reddy, Kappari. Sharadha Devi. A novel method for determination of Tetracycline and its metabolite residues in cow milk. Research Journal of Pharmacy and Technology. 2014; 7(5): 513-516. Available on: https://rjptonline.org/AbstractView.aspx?PID=2014-7-5-15
12. Vishnuraj MR, Kandeepan G, Rao KH, Chand S, Kumbhar V. Occurrence, public health hazards and detection methods of antibiotic residues in foods of animal origin: A comprehensive review. Cogent Food & Agriculture. 2016; 2(1). Available from: http://dx.doi.org/10.1080/23311932.2016.1235458
13. Trouchon T, Lefebvre S. A review of enrofloxacin for veterinary use. Open Journal of Veterinary Medicine. 2016; 06(02): 40–58. Available from: http://dx.doi.org/10.4236/ojvm.2016.62006
14. Papich MG. Saunders handbook of veterinary drugs: Small and large animal. 4th ed. Philadelphia, PA: Saunders; 2015.
15. Elmahadii TO, Shantier SWA, Adam ME. Development and Validation of UV-Spectrophotometric method for the Determination of Enrofloxacin in Synthetic form and Veterinary Injectible Dosage forms. Asian Journal of Pharmaceutical Analysis. 2019; 9(1): 11. Available from: http://dx.doi.org/10.5958/2231-5675.2019.00004.8
16. Ajay Gadgul, Ramling Patarkar, Kamlesh Niranjane, Anant Deshpande, Sandeep Walsangikar. Quinolones Chemistry and its Therapeutic Activities. Research Journal of Pharmacy and Technology. 2010; 3 (4): Oct.-Dec. 1023-1028.
17. Baytril 2.5% injectable, Baytril 5% injectable and Baytril 10% injectable and their associated names, and related veterinary medicinal products: Annex I, II, III. Europa.eu. [cited 2024 Jul 27]. Available from: https://www.ema.europa.eu/en/documents/referral/baytril-25-injectable-baytril-5-injectable-and-baytril-10-injectable-and-their-associated-names-and-related-veterinary-medicinal-products-annex-i-ii-iii_en.pdf
18. 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. Europa.eu. [cited 2024 Jul 27]. Available from: https://health.ec.europa.eu/document/download/f96d367d-45f8-474c-a513-2ac667f5dd13_en
19. Residues of some veterinary drugs in foods and animals. Fao.org. [cited 2024 Jul 27]. Available from: https://www.fao.org/food/food-safety-quality/scientific-advice/jecfa/jecfa-vetdrugs/details/en/c/63/
20. Evaluations of the Joint FAO/WHO Expert Committee on Food Additives (JECFA). Who.int. [cited 2024 Jul 27]. Available from: https://apps.who.int/food-additives-contaminants-jecfa-database/Home/Chemical/597
21. Alfonseca-Silva E, Cruz-Villa JC, Gutiérrez L, Sumano H. Successful treatment of recurrent subclinical mastitis in cows caused by enrofloxacin resistant bacteria by means of the sequential intramammary infusion of enrofloxacin HCl-2H2O and ceftiofur HCl: a clinical trial. Journal of Veterinary Science. 2021; 22(6). Available from: http://dx.doi.org/10.4142/jvs.2021.22.e78
22. Martínez-Cortés I, Gutierrez L, Tapia G, Ocampo L, Sumano H. Serum and milk concentrations of enrofloxacin in cows intramammarily treated with a new enrofloxacin-polymorph. Med Weter. 2016; 72(11): 686–92. Available from: http://dx.doi.org/10.21521/mw.5587
23. Idowu OR, Peggins JO. Simple, rapid determination of enrofloxacin and ciprofloxacin in bovine milk and plasma by high-performance liquid chromatography with fluorescence detection. Journal of Pharmaceutical and Biomedical Analysis. 2004;35(1):143–53. Available from: http://dx.doi.org/10.1016/j.jpba.2004.01.006
24. Moudgil P, Bedi JS, Aulakh RS, Gill JPS, Kumar A. Validation of HPLC multi-residue method for determination of fluoroquinolones, tetracycline, sulphonamides and chloramphenicol residues in bovine milk. Food Analytical Methods. 2019; 12(2): 338–46. Available from: http://dx.doi.org/10.1007/s12161-018-1365-0
25. Cinquina AL, Roberti P, Giannetti L, Longo F, Draisci R, Fagiolo A, et al. Determination of enrofloxacin and its metabolite ciprofloxacin in goat milk by high-performance liquid chromatography with diode-array detection. Journal of Chromatography A. 2003; 987(1–2): 221–6. Available from: https://pubmed.ncbi.nlm.nih.gov/12613815/
26. Filip C, Ceanăă D-E, Vescan AT. HPLC method with fluorescence detection for the identification and quantitative determination of fluoroquinolones in milk. Amtsibiu.ro. [cited 2024 Jul 27]. Available from: http://amtsibiu.ro/Arhiva/2014/Nr1-en/Filip-Ceana-en.pdf
27. Tang Q, Yang T, Tan X, Luo J. Simultaneous determination of fluoroquinolone antibiotic residues in milk sample by solid-phase Extraction−Liquid Chromatography−Tandem mass spectrometry Journal of agricultural and food chemistry. 2009; 57(11): 4535–9. Available from: http://dx.doi.org/10.1021/jf900513b
28. Choma I. Screening of enrofloxacin and ciprofloxacin residues in milk by HPLC and by TLC with direct bioautography. JPC–Journal of Planar Chromatography–Modern TLC. 2006; 19(108): 104–8. Available from: http://dx.doi.org/10.1556/jpc.19.2006.2.3
29. Parmar A, Sharma S. Derivative UV-vis absorption spectra as an invigorated spectrophotometric method for spectral resolution and quantitative analysis: Theoretical aspects and analytical applications: A review. TrAC Trends in Analytical Chemistry. 2016; 77: 44–53. Available from: http://dx.doi.org/10.1016/j.trac.2015.12.004
30. J. Vyas A, M. Vadile H, I. Patel A, B. Patel A, V. Dudhrejiya A, R. Shah S, et al. Recent applications of UV-visible derivative spectroscopic method. Asian Journal of Pharmaceutical Analysis. 2023; 108–14. Available from: http://dx.doi.org/10.52711/2231-5675.2023.00019
31. ICH Harmonised Tripartite Guideline. International conference on harmonisation of technical requirements for registration of pharmaceuticals for human use. Ich.org. [cited 2024 Jul 27]. Available from: https://database.ich.org/sites/default/files/Q2%28R1%29%20Guideline.pdf
32. Guidance for Industry Studies to Evaluate the Metabolism and Residue Kinetics of Veterinary Drugs in Food-Producing Animals: Validation of Analytical Methods. Used in Residue Depletion Studies. fda.gov. [cited 2024 Jul 27]. Available from: https://www.fda.gov/media/78356/download