title: Analysis of amprolium by hydrophilic interaction liquid chromatography-tandem mass spectrometry.
abstract: We present a fast liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the analysis of the coccidiostat amprolium in food samples. Tandem mass spectrometry in a triple quadrupole was used for quantitative purposes, and the information from multiple-stage mass spectrometry in an ion-trap mass analyzer contributed to fragmentation studies. Hydrophilic interaction liquid chromatography (HILIC) in a Fused-Core column using isocratic elution (acetonitrile:formic acid/ammonium formate buffer pH 4, 50 mM (60:40)) successfully analyzed this compound in less than 3 min. The HILIC system was coupled to heated electrospray-MS/MS using highly selective-selected reaction monitoring (H-SRM) to improve sensitivity and selectivity for the analysis of amprolium, after a simple sample treatment based on an "extract and shoot" strategy. Accurate mass measurements were performed to identify the interfering compound responsible for causing matrix ion enhancement in the signal of amprolium. The addition of l-carnitine (the interfering compound) (1 microg L(-1)) to standards and sample extracts allowed the use of the external calibration method for quantitative purposes. The LC-MS/MS (H-SRM) method showed good precision (relative standard deviation, RSD, lower than 13%), accuracy and linearity and allowed the determination of amprolium down to the ppb level (LODs between 0.1 and 0.6 microg kg(-1)).
authors.affiliation: Department of Analytical Chemistry, University of Barcelona, Martí i Franquès 1-11, E-08028 Barcelona, Spain.
authors.forename: Anna
authors.initials: A
authors.lastname: Martínez-Villalba
authors.forename: Encarnación
authors.initials: E
authors.lastname: Moyano
authors.forename: M Teresa
authors.initials: MT
authors.lastname: Galceran
mesh_terms: D000670:Amprolium / Q000032:analysis*; D000818:Animals; D002331:Carnitine / Q000032:analysis; D002645:Chickens; D002853:Chromatography, Liquid / Q000379:methods*; D003049:Coccidiostats / Q000032:analysis; D004531:Eggs / Q000032:analysis; D005504:Food Analysis / Q000379:methods*; D006863:Hydrogen-Ion Concentration; D057927:Hydrophobic and Hydrophilic Interactions; D016014:Linear Models; D008460:Meat / Q000032:analysis; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D003049:Coccidiostats; D000670:Amprolium; D002331:Carnitine