Ulaş ACARÖZ, Sinan İNCE, Recep KARA, Zeki GÜRLER, Damla ARSLAN ACARÖZ, İsmail KÜÇÜKKURT, Abdullah ERYAVUZ

Anadolu manda sütündeki enrofloksasin atılımının değerlendirilmesi

Enrofloksasin (ENR), hem beşeri hekimlikte hem de veteriner hekimlikte yaygın olarak kullanılan geniş spektrumlu bir florokinolon antibiyotiktir. Bu çalışmada laktasyondaki mandalara ENR'nin (2,5 mg/kg vücut ağırlığı) intramusküler uygulamasını takiben 10. sağımına kadar ENR ve metaboliti siprofloksasinin (CIP) süt ile atılımı belirlendi. Her bir hayvanın sütü toplanarak ENR ve CIP düzeyleri LC-MS/MS ile tespit edildi. Yöntemin tespit sınırları ENR ve CIP için sırasıyla 0,35 μg/kg ve 0,12 μg/kg olarak saptandı. ENR ve metaboliti CIP'nin en yüksek toplam düzeyleri, enjeksiyondan sonraki ikinci sağımda 603 μg/kg olarak tespit edildi. Tüm manda sütü numunelerindeki kalıntı seviyesinin, beşinci sağımda maksimum kalıntı limitinden (100 μg/kg) daha düşük olduğu belirlendi. Ayrıca, kullanılan yöntem, tüketime sunulan 50 manda sütü örneğinde ENR ve CIP kalıntı varlığını değerlendirmek içinbaşarılı bir şekilde uygulandı ve hiçbir örneğinin bu antibiyotikleri içermediği saptandı. Sonuç olarak bu çalışma, LC-MS/MS yöntemi kullanılarak Anadolu mandalarında ENR ve CIP'in süt atılım seviyeleri hakkında bilgi sağladı. Anahtar sözcükler: Anadolu mandası, atılım, enrofloksasin, LC-MS/MS, siprofloksasin, süt.

Evaluation of the enrofloxacin excretion in Anatolian buffalo milk

Enrofloxacin (ENR) is a broad-spectrum fluoroquinolone antibiotic widely used in both human medicine and veterinary medicine. In this study, the milk-excretion patterns of ENR and its metabolite ciprofloxacin (CIP) were determined up to the 10th milking following the intramuscular administration of ENR (2.5mg/kg of body weight) to lactating dairy buffaloes. The milk of each animal was collected and the concentrations of ENR and CIP were detected in milk by LC-MS/MS. The detection limits of the method were determined for ENR and CIP as 0.35 μg/kg and 0.12 μg/kg, respectively. The highest total mean concentrations of ENR and its metabolite CIP was determined in the second milking after injection as 603 μg/kg. The residue level in all buffalo milk samples was found to be lower than the maximum residue limit (100 μg/kg) at the fifth milking. In addition, the employed method is successfully applied to evaluate the presence of ENR and CIP residue in 50 marketed buffalo milk samples and none of the samples contained these antibiotics. Consequently, the present study provided information on the milk excretion levels of ENR and CIP in Anatolian buffalo milks by an LC-MS/MS method.

PDF

___

1. Acaroz U, Arslan-Acaroz D, Ince S (2019): A Wide Perspective on Nutrients in Beverages. 1-39. In: Grumezescu AM and Holban AM (Ed) Nutrients in Beverages. Academic Press.
2. Acaroz U, Dietrich R, Knauer M, et al (2019): Development of a Generic Enzyme-Immunoassay for the Detection of Fluoro(quinolone)-Residues in Foodstuffs Based on a Highly Sensitive Monoclonal Antibody. Food Anal Methods, 13, 780-792.
3. Acaroz U, Ince S, Arslan-Acaroz D, et al (2020): Determination of kanamycin residue in anatolian buffalo milk by LC-MS/MS. Kafkas Univ Vet Fak Derg, 26, 97–102.
4. Chui-Shiang C, Wei-Hsien W, Chin-En T (2010): Simultaneous Determination of 18 Quinolone Residues in Marine and Livestock Products by Liquid Chromatography/ Tandem Mass Spectrometry. J Food Drug Anal, 18, 87–97.
5. Cinquina AL, Roberti P, Giannetti L, et al (2003): Determination of enrofloxacin and its metabolite ciprofloxacin in goat milk by high-performance liquid chromatography with diode-array detection: Optimization and validation. J Chromatogr A, 987, 221-226.
6. Cuypers WL, Jacobs J, Wong V, et al (2018): Fluoroquinolone resistance in Salmonella: Insights by wholegenome sequencing. Microb Genomics, 4, e000195.
7. Du C, Deng T, Zhou Y, et al (2019): Systematic analyses for candidate genes of milk production traits in water buffalo (Bubalus Bubalis). Anim Genet, 50, 207–216.
8. EU Commission Regulation (2019): Pharmacologically active substances and their classification regarding maximum residue limits in foodstuffs of animal origin. Available at https://ec.europa.eu/health/sites/health/files/files/eudralex/vol-5/reg_2010_37/reg_2010_37_en.pdf.(Accessed January 20, 2020).
9. Haritova A, Lashev L, Pashov D (2003):Pharmacokinetics of enrofloxacin in lactating sheep. Res Vet Sci, 74, 241–245.
10. Idowu OR, Peggins JO (2004): Simple, rapid determination of enrofloxacin and ciprofloxacin in bovine milk and plasma by high-performance liquid chromatography with fluorescence detection. J Pharm Biomed Anal, 35, 143–153.
11. Jank L, Martins MT, Arsand JB, et al (2015): Highthroughput method for the determination of residues of βlactam antibiotics in bovine milk by LC-MS/MS. Food Addit Contam - Part A Chem Anal Control Expo Risk Assess, 32, 1992–2001.
12. Kaartinen L, Salonen M, Älli L, et al (1995): Pharmacokinetics of enrofloxacin after single intravenous, intramuscular and subcutaneous injections in lactating cows. J Vet Pharmacol Ther, 18, 357–362.
13. Kara R, Acaroz U, Gurler Z, et al (2018): Manda Sütlerinde ICP-MS ile Metal ve Ağır Metal Seviyelerinin Belirlenmesi. Kocatepe Vet J, 11, 1–4.
14. Lei Z, Liu Q, Yang B, et al (2017): Clinical efficacy and residue depletion of 10% enrofloxacin enteric-coated granules in pigs. Front Pharmacol, 8, 1–11.
15. Lizondo M, Pons M, Gallardo M, et al (1997): Physicochemical properties of enrofloxacin. J Pharm Biomed Anal, 15, 1845–1849.
16. Lv YK, L Yang, XH Liu, et al (2013): Preparation and evaluation of a novel molecularly imprinted hybrid composite monolithic column for on-line solid-phase extraction coupled with HPLC to detect trace fluoroquinolone residues in milk. Anal Methods, 5, 1848–1855.
17. Mahmood T, Abbas M, Ilyas S, et al (2016):Quantification of fluoroquinolone (enrofloxacin, norfloxacin and ciprofloxacin) residues in cow milk. IJCBS, 10, 10–15.
18. Malbe M, Salonen M, Fang W, et al (1996): Disposition of enrofloxacin (Baytril) into the udder after intravenous and intra-arterial injections into dairy cows. J Vet Med A, 43, 377–386.
19. Mohammed HA, Abdou AM, Eid AM, et al (2016): Rapid tests for detection of enrofloxacin residues in liquid milk. Benha Vet Med J, 30, 97–103.
20. Naeem A, Badshah SL, Muska M, et al (2016): The current case of quinolones: Synthetic approaches and antibacterial activity. Molecules, 21, 268.
21. Nirala RK, Anjana K, Mandal KG, et al (2017): Persistence of antibiotic residue in milk under region of Bihar, India. Int J Curr Microbiol App Sci, 6, 2296–2299.
22. Piñero MY, Fuenmayor M, Arce L, et al (2013): A simple sample treatment for the determination of enrofloxacin and ciprofloxacin in raw goat milk. Microchem J, 110, 533–537.
23. Rath S, Padhy RN (2015): Prevalence of fluoroquinolone resistance in Escherichia coli in an Indian teaching hospital and adjoining communities. J Taibah Univ Med Sci, 10, 504–508.
24. Sierra-Arguello YM, Furian TQ, Perdoncini G, et al(2018): Fluoroquinolone resistance in Campylobacter jejuni and Campylobacter coli from poultry and human samples assessed by PCR-restriction fragment length polymorphism assay. PLoS One, 13, 1–9.
25. Talpade J (2018): pharmacokinetic study of single dose intravenous administration of enrofloxacin in Barbari goats. J Anim Res, 8, 609–611.
26. Tian H (2011): Determination of chloramphenicol, enrofloxacin and 29pesticides residues in bovine milk by liquid chromatography-tandem mass spectrometry. Chemosphere, 83, 349–355.
27. Tian Z, Gao JJ, Qin W (2018): Determination of fluoroquinolones in milk by ionic liquid-mediated two phaseextraction followed by capillary electrophoresis analysis. Madridge J Anal Sci Instrum, 3, 62–67.
28. Trouchon T, Lefebvre S (2016): A review of enrofloxacin for veterinary use. Open J Vet Med, 6, 40–58.
29. Ziv G (1994): Pharmacokinetics of Antibacterial Fluoroquinolones in Small and Large Animal Practice. 194-196. In: Proceedings of the 6th Congress of EAVPT Congress, Edinburgh.