Investigation of the persistence of rafoxanide residues in bovine milk and fate during processing

Abstract

Rafoxanide is an effective treatment for the control of fluke infections in animals, but it is currently not permitted for treating animals whose milk is intended for human consumption. In this study, the persistence of rafoxanide residues in milk, and their migration to dairy products, was investigated following the treatment of six lactating dairy cows with Curafluke 10% oral drench. The highest concentration of rafoxanide residues detected in the individual cows milk ranged from 249 to 627 μg kg⁻¹ and occurred at 2–3 days post-treatment. At 2 and 23 days post-treatment (representing high and low residue concentrations) the milk was pooled into two independent aliquots, each containing the full day’s milk produced by three cows. Milk products were made from pasteurised and unpasteurised milk. Pasteurisation appeared to have little impact on the stability of the residues. Rafoxanide concentrated sixfold in the cheese (week 0) compared to the starting milk (2070 vs. 349 μg kg⁻¹) but was four times lower in whey (75 μg kg⁻¹). Rafoxanide residues were up to 14 times higher in butter (week 0) than in the starting milk (5468 vs. 376 μg kg⁻¹). Residues were found to further concentrate in butter and cheese at longer storage and ripening times, respectively. Skim-milk powder was manufactured from skim milk, and residues were 10-fold higher than in the starting skim milk (5468 vs. 376 μg kg⁻¹) despite the 185°C temperature required for the process. Rafoxanide residues were stable in this skim-milk powder when stored at ambient temperature for at least 1 year. Results showed that detectable rafoxanide residues were excreted in milk for 47 days, and concentrated in the fat-based products. The analytical ranges of the UHPLC-MS/MS method used were 1.0–200 μg kg⁻¹ (milk and whey) and 10–2000 μg kg⁻¹ (other dairy products).

Keywords:

• rafoxanide
• salicylanilide
• anthelmintic
• flukicide
• residues
• milk
• dairy products
• cheese
• whey
• skim milk
• powder
• UHPLC-MS/MS

Acknowledgements

This work was supported by the Dairy Levy Trust. The authors acknowledge the staff at Ashtown, in particular Martin McCormack, and the farm staff at Moorepark, in particular Noel Byrne and John Paul Murphy, for their valuable assistance. Clare Power was in receipt of a Teagasc Walsh Fellowship.