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Development and validation of two multiresidue liquid chromatography tandem mass spectrometry methods based on a versatile extraction procedure for isolating non-steroidal anti-inflammatory drugs from bovine milk and muscle tissue

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Abstract

The main difficulties in analysing non-steroidal anti-inflammatory drugs (NSAIDs) in food and biological samples are due to the tight non-covalent interactions established with matrix proteins and the amount of occurring fatty material. The present paper describes an effective extraction procedure able to isolate fifteen NSAIDs (acetaminophen, salicylic acid, ibuprofen, diclofenac, flunixin and its metabolite 5-hydroxy-flunixin, nimesulide, phenylbutazone, meclofenamic acid, tolfenamic acid, meloxicam, carprofen, ketoprofen, naproxen and etodolac) from bovine milk and muscle tissue through two succeeding steps: (a) deproteinisation/extraction with organic solvent, essential to lower the medium dielectric constant and, therefore, to release the analytes from matrix; (b) SPE clean-up on OASIS cartridges. Lipids were easily removed during low-temperature centrifugations. The advantages of the developed procedure pertain to the efficient removal of the fat substances (very low matrix effect and high recovery yields) and its versatility, since it can be applied both to milk and muscle with few adjustments due to the diversity of the two matrices. Ion-pairing reversed-phase chromatography combined with the negative electrospray detection was able to achieve low detection capabilities (CCβs) for all analytes and, in particular, for diclofenac whose Maximum Residue Limit (MRL) in milk is 0.1 μg kg−1. The methods were validated according to the guidelines of the Commission Decision 2002/657/EC and then applied for a small monitoring study. A number of samples showed traces of salicylic acid (SA), but its occurrence was not ascribed to a misuse of drugs (aspirin, salicylic acid) since SA, accumulating in plants in response to a pathogen attack, may be introduced into the food chain.

Figurative representation of NSAIDs contamination in milk

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Acknowledgements

The authors would like to thank Dr. Bruno Neri for his helpful suggestions.

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Authors and Affiliations

  1. Department of Chemistry, Faculty of Mathematical, Physical and Natural Sciences, “Sapienza” University of Rome, P.le A. Moro no. 5, P.O. Box 34, Posta 62, 00185, Rome, Italy

    Alessandra Gentili, Fulvia Caretti, Simona Bellante, Roberta Curini & Alessandro Venditti

  2. Italian Workers’ Compensation Authority (INAIL)—ISPESL Area, Department of Occupational Hygiene, Laboratory of Chemical Agents, Via Fontana Candida 1, 00040, Monte Porzio Catone, Rome, Italy

    Lucia Mainero Rocca

Authors
  1. Alessandra Gentili
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  2. Fulvia Caretti
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  3. Simona Bellante
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  4. Lucia Mainero Rocca
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  5. Roberta Curini
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  6. Alessandro Venditti
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Correspondence to Fulvia Caretti.

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Gentili, A., Caretti, F., Bellante, S. et al. Development and validation of two multiresidue liquid chromatography tandem mass spectrometry methods based on a versatile extraction procedure for isolating non-steroidal anti-inflammatory drugs from bovine milk and muscle tissue. Anal Bioanal Chem 404, 1375–1388 (2012). https://doi.org/10.1007/s00216-012-6231-0

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  • DOI: https://doi.org/10.1007/s00216-012-6231-0

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