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Food Analytical Methods

, Volume 10, Issue 7, pp 2490–2496 | Cite as

Determination of Diclofenac in Bovine Milk at Low Levels Using Ultra High Performance Liquid Chromatography–Tandem Mass Spectrometry

Article

Abstract

This paper reports on the development and validation of a simple, rapid, and sensitive ultra high performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method to quantify low levels of diclofenac in bovine milk samples. The sample preparation procedure involves the milk deproteination by ethyl acetate in the presence of sodium acetate and silica at pH = 4.0 adjusted with acetic acid. The extract was evaporated, reconstituted, and injected into a chromatographic system prior to the analysis, which used a C18 column and mobile phase gradient elution. Data were acquired under MS tandem using positive electrospray (ESI) mode and multiple reaction monitoring (MRM). The calibration curve was linear across the concentration range of 0.05–5.00 ng mL−1 with LOD and LOQ of 0.015 and 0.048 ng mL−1, respectively. The proposed method provides acceptable values for repeatability (RSD < 18.8%), intermediary precision (RSD < 15.3%), and accuracy (−2.3–14.9%).

Keywords

Diclofenac Bovine milk Residues UHPLC–MS/MS 

Notes

Acknowledgments

The authors are grateful to Alcimar C. Valerio (in memoriam) for helpful discussion in the early stages of the sample preparation steps.

This work was supported by the Coordination for the Improvement of Higher Education Personnel (CAPES), the São Paulo Research Foundation (FAPESP) under grant 2005/59360-0, the Brazilian National Council for Scientific and Technological Development (CNPq) under grant 306685/2009-4 and 162528/2013-2, and the Brazilian Innovation Agency (FINEP) under grant 01.08235-01.

Compliance with Ethical Standards

The authors declare that this manuscript corresponds to an original research article not published before neither presently submitted for publication elsewhere.

Funding

This work was supported by the Coordination for the Improvement of Higher Education Personnel (CAPES), the São Paulo Research Foundation (FAPESP) under grant 2005/59360-0, the Brazilian National Council for Scientific and Technological Development (CNPq) under grant 306685/2009-4 and 162528/2013-2, and the Brazilian Innovation Agency (FINEP) under grant 01.08235-01.

Conflict of Interest

Carlos E. D. Nazario declares that he has no conflict of interest. Fernando M. Lancas declares that he has no conflict of interest.

Ethical Approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Informed Consent

Not applicable.

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Copyright information

© Springer Science+Business Media New York 2017

Authors and Affiliations

  1. 1.Institute of ChemistryFederal University of Mato Grosso do SulCampo GrandeBrazil
  2. 2.Institute of Chemistry of Sao CarlosUniversity of Sao PauloSao CarlosBrazil

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