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Development and validation of an UPLC-MS/MS method for the determination of ionophoric and synthetic coccidiostats in vegetables

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Abstract

In poultry farming, anticoccidial drugs are widely used as feed additives for the prevention and treatment of coccidiosis. Because coccidiostats and veterinary medicines, in general, are often poorly absorbed, manure from treated animals may contain high concentrations of these compounds. Experimental studies have shown that the uptake of veterinary medicines by plants from soil containing contaminated manure may occur. This leads to several questions regarding the impact on the environment, resistance problems, and public health and allergy issues. This work describes the development of a quantification method for coccidiostats in vegetables. Vegetables were spiked at 100 μg kg−1 (dry weight) with coccidiostats (monensin, narasin, lasalocid A, salinomycin, diclazuril, and nicarbazin) in order to optimize the extraction and clean-up. Possible critical factors (e.g., extraction solvent) were statistically examined by linear regression with the use of Plackett–Burman and full factorial designs. Final extracts were analyzed with ultra-performance liquid chromatography tandem mass spectrometry operating in multiple-reaction monitoring mode. Both the synthetic and ionophoric coccidiostats could be determined in a single run with an analysis time of 5 min. The developed method was validated taking into account the requirements of the Commission Decision 2002/657/EC as a guideline. The method is regarded as applicable for its intended purposes with quantification limits between 0.30 and 2.98 μg kg−1. This method could be used to establish possible maximum residue limits for coccidiostats in vegetables, as already exist for eggs, meat, and milk.

Chromatogram of a 10 μg kg−1 spiked, freeze-dried carrot sample; X: Carrot-specific interference in the channel of dinitrocarbanilide (DNC); A: DNC; B: diclazuril; C: monensin; D: lasalocid A; E: salinomycin; F: narasin

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Acknowledgments

We are grateful to the European Food Safety Authority (EFSA) for the project funding (CFP/EFSA/CONTAM/2010/02). This paper is produced by the bodies identified above as authors; it is not produced by EFSA. EFSA reserves its right, view, and position as regards the issues addressed and conclusions reached in the present document, without prejudice to the rights of the authors.

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Authors and Affiliations

  1. Department of Bioanalysis, Laboratory of Food Analysis, Ghent University, Harelbekestraat 72, 9000, Ghent, Belgium

    N. Broekaert, C. Van Peteghem, D. Sticker & C. Van Poucke

  2. Technology and Food Science Unit, Institute for Agricultural and Fisheries Research (ILVO), Brusselsesteenweg 370, 9090, Melle, Belgium

    E. Daeseleire

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  1. N. Broekaert
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  2. C. Van Peteghem
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  3. E. Daeseleire
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  4. D. Sticker
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  5. C. Van Poucke
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Correspondence to N. Broekaert.

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Broekaert, N., Van Peteghem, C., Daeseleire, E. et al. Development and validation of an UPLC-MS/MS method for the determination of ionophoric and synthetic coccidiostats in vegetables. Anal Bioanal Chem 401, 3335–3344 (2011). https://doi.org/10.1007/s00216-011-5433-1

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  • DOI: https://doi.org/10.1007/s00216-011-5433-1

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