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Separations 2017, 4(2), 15; doi:10.3390/separations4020015

Liquid Chromatography Tandem Mass Spectrometry Analysis of Synthetic Coccidiostats in Eggs

1
Department of Chemistry, University ”Sapienza”, P.le Aldo Moro, 5-0185 Rome, Italy
2
Inail DIT—Via Roberto Ferruzzi, 38-00143 Rome, Italy
3
Istituto Zooprofilattico e Sperimentale Regioni Lazio e Toscana—Via Appia Nuova, 1411-00178 Rome, Italy
*
Author to whom correspondence should be addressed.
Academic Editor: Michael J. Dunphy
Received: 4 January 2017 / Revised: 21 February 2017 / Accepted: 29 March 2017 / Published: 17 April 2017
(This article belongs to the Special Issue Advances in High Pressure Liquid Chromatography)
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Abstract

Coccidiostats are synthetic drugs administered to animals, especially to poultry, to cure coccidiosis. In this paper, we present a selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to analyze residues of five synthetic coccidiostats in eggs: clazuril, diclazuril, robenidine, nicarbazin, toltrazuril and its two metabolites. The extraction efficiency was evaluated by testing several solvents, pH, different volumes and time of extraction. The clean-up procedures were optimized using different solid phase extraction cartridges and different eluants. The chromatographic separation was achieved in reversed phase using a gradient of 0.1% formic acid in water and acetonitrile, whereas the MS detection was performed in negative electrospray ionization (ESI) for all the analytes, except for the robenidine. The developed method has been validated according to Commission Decision 2002/657/CE. The validation parameters, as linearity, precision, recovery, specificity, decision limit (CCα), detection capability (CCβ), and robustness have been determined. The proposed method resulted simple, fast, and suitable for screening and confirmation purposes. View Full-Text
Keywords: synthetic coccidiostats; eggs; mass spectrometry synthetic coccidiostats; eggs; mass spectrometry
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MDPI and ACS Style

Buiarelli, F.; Di Filippo, P.; Riccardi, C.; Pomata, D.; Giannetti, L.; Neri, B.; Rago, D. Liquid Chromatography Tandem Mass Spectrometry Analysis of Synthetic Coccidiostats in Eggs. Separations 2017, 4, 15.

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