title: Development and validation of a liquid chromatographic-tandem mass spectrometric method for determination of eleven coccidiostats in milk.
abstract: A reversed phase liquid chromatographic-tandem mass spectrometric method with simple solvent extraction and purification by solid phase extraction (SPE) has been developed for the determination of coccidiostats in milk. For sample preparation matrix solid phase dispersion, extraction by organic solvent and SPE with different cartridges were also tested. The compounds determined include lasalocid, narasin, salinomycin, monensin, semduramicin, maduramicin, robenidine, decoquinate, halofuginone, nicarbazin and diclazuril. Main steps of the method are addition of acetonitrile to the milk samples, centrifugation, removal of matrix by SPE, concentration by evaporation and LC-MS-MS determination. During a 15 min time segmented chromatographic run compounds are ionised either positively or negatively. Calculated recoveries range between 77.1% and 118.2%. Maximum levels are in the range of 1-20 μg/kg. The developed method was validated in line with the requirements of Commission Decision 2002/657/EC (2002). It is applicable for control of coccidiostat residues in milk as indicated in Regulation 124/2009/EC (2009).
authors: Joint Research and Training Laboratory on Separation Techniques, Eötvös Loránd University, 1117 Budapest, Pázmány Péter Sétány 1/A, Hungary. Electronic address: szilard.nasz@gmail.com.
authors: Szilárd
authors: S
authors: Nász
authors: Central Agricultural Office, Food and Feed Safety Directorate, Feed Investigation National Reference Laboratory, 1144 Budapest, Remény utca 42, Hungary.
authors: Lajos
authors: L
authors: Debreczeni
authors: Wessling International Research and Educational Center, 1047 Budapest, Fóti út 56, Hungary.
authors: Tamás
authors: T
authors: Rikker
authors: Joint Research and Training Laboratory on Separation Techniques, Eötvös Loránd University, 1117 Budapest, Pázmány Péter Sétány 1/A, Hungary; Wessling International Research and Educational Center, 1047 Budapest, Fóti út 56, Hungary. Electronic address: eke.zsuzsanna@wirec.eu.
authors: Zsuzsanna
authors: Z
authors: Eke
mesh_terms: D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods*; D003049:Coccidiostats / Q000032:analysis*; D008892:Milk / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D003049:Coccidiostats
keywords: Coccidiostats; LC–MS–MS; Milk; Solid phase extraction; Validation