title: Investigation of the persistence of nitroxynil residues in milk from lactating dairy cows by ultra performance liquid chromatography tandem mass spectrometry.
abstract: Nitroxynil is an anthelmintic used in the treatment of liver fluke. In this study, six dairy cows were treated during lactation with Trodax, a 34% solution containing nitroxynil as its N-ethylglucamine salt, indicated for the treatment of fascioliasis in cattle and sheep. Samples were collected twice daily for 16 days and later at weekly intervals up to 58 days post-treatment. Nitroxynil residues were extracted from milk samples using acetonitrile; magnesium sulfate and sodium chloride were added to induce liquid-liquid partitioning and purified by dispersive solid phase extraction for clean-up. Nitroxynil was determined by ultra performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) in negative ionization mode. The limit of detection (CCα) of the method is 0.24 μg/kg. Maximum concentration of nitroxynil in the samples was in the range of 688-1358 μg/kg, with levels persisting for 58 days in four of the six lactating cows. Incurred nitroxynil samples were treated with sulfatase and β-glucuronidase from Helix pomatia ; the results indicated the presence of glucuronide conjugates in samples at early withdrawal times. At later withdrawal times the concentration of free nitroxynil was lower than the concentration in the control samples, indicating potential degradation during enzymatic treatment.
authors.affiliation: Food Safety Department, Teagasc Food Research Centre, Ashtown, Dublin 15, Ireland.
authors.forename: Michelle
authors.initials: M
authors.lastname: Whelan
authors.forename: Yris
authors.initials: Y
authors.lastname: Bloemhoff
authors.forename: Ambrose
authors.initials: A
authors.lastname: Furey
authors.forename: Riona
authors.initials: R
authors.lastname: Sayers
authors.forename: Martin
authors.initials: M
authors.lastname: Danaher
mesh_terms: D000818:Animals; D000871:Anthelmintics / Q000032:analysis* / Q000627:therapeutic use; D002417:Cattle; D002418:Cattle Diseases / Q000188:drug therapy / Q000503:physiopathology; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis*; D005211:Fascioliasis / Q000188:drug therapy / Q000503:physiopathology / Q000662:veterinary*; D005260:Female; D005506:Food Contamination / Q000032:analysis; D007774:Lactation; D008892:Milk / Q000737:chemistry*; D009611:Nitroxinil / Q000032:analysis* / Q000627:therapeutic use; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D000871:Anthelmintics; D009611:Nitroxinil