title: Determination of eleven coccidiostats in animal feed by liquid chromatography-tandem mass spectrometry at cross contamination levels.
abstract: A confirmatory multi-residue method has been developed to allow for the detection, confirmation and quantification of eleven coccidiostats in animal feed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method can be used to determine halofuginone, robenidine, nicarbazin, diclazuril, decoquinate, semduramicin, lasalocid, monensin, salinomycin, narasin, maduramicin at levels relating to unavoidable carry over as stated in Regulation 2009/8/EC. Feed samples are extracted with water and acetonitrile with the addition of anhydrous magnesium sulphate and sodium chloride. The extract then undergoes a freezing out step before being diluted and injected onto the LC-MS/MS system. The LC-MS/MS system is run in MRM mode with both positive and negative electrospray ionisation and can confirm all eleven analytes in a run time of 19 min. The sensitivity of the method allows quantification and confirmation for all coccidiostats at a 0.5% carry over level. The method was validated over three days in accordance with of European legislation; Commission Decision 2002/657/EC. Validation criteria of accuracy, precision, decision limit (CCα), and detection capability (CCβ) along with measurement uncertainty are calculated for all analytes. The method was then successfully used to analyse a number of feed samples that contained various coccidiostat substances.
authors: School of Pharmaceutical and Chemical Sciences, Dublin Institute of Technology, Dublin, Ireland. mark.cronly@statelab.ie
authors: Mark
authors: M
authors: Cronly
authors: P
authors: P
authors: Behan
authors: B
authors: B
authors: Foley
authors: E
authors: E
authors: Malone
authors: P
authors: P
authors: Shearan
authors: L
authors: L
authors: Regan
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D000821:Animal Feed / Q000032:analysis*; D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003049:Coccidiostats / Q000032:analysis*; D008278:Magnesium Sulfate / Q000737:chemistry; D012965:Sodium Chloride / Q000737:chemistry; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014867:Water / Q000737:chemistry
chemical_list: D000097:Acetonitriles; D003049:Coccidiostats; D014867:Water; D012965:Sodium Chloride; D008278:Magnesium Sulfate; C032159:acetonitrile