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A confirmatory method for the determination of phenolic endocrine disruptors in honey using restricted-access material–liquid chromatography–tandem mass spectrometry

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Abstract

The present work describes the development and validation of an analytical method based on liquid chromatography (LC), coupled with tandem mass spectrometry (MS/MS) that allows the determination and confirmation of several endocrine-disrupting chemicals (EDCs) in honey. The EDCs studied were nine phenols of different nature: chlorophenols (2,4-dichlorophenol, 2,4,5-trichlorophenol, and pentachlorophenol), alkylphenols (4-tert-butylphenol, 4-tert-octylphenol, and 4-n-octylphenol) bisphenols (bisphenol-A and bisphenol-F), and 4-tert-butylbenzoic acid. The method incorporates a restricted-access material (RAM), coupled on-line to the LC-MS/MS system, which allows direct injection of the matrix into the RAM-LC-MS/MS system. The optimized method developed, RAM-LC-MS/MS, was applied to fortified honey samples, affording detection limits in the 0.6–7.2 ng g−1 range, calculated for a signal-to-noise ratio of 3. In addition, the method was validated as a quantitative confirmatory method according to European Union Decision 2002/657/EC. The validation criteria evaluated were linearity, repeatability, reproducibility, recovery, decision limits, detection capabilities, specificity, and ruggedness. Repeatability and within-laboratory reproducibility were evaluated at two concentration levels, being ±11% or below at 20 ng g−1. The decision limits (CCα) and detection capabilities (CCβ) were in the 1.7–12.6 and 2.8–21.6 ng g−1 range, respectively.

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Acknowledgments

The Ministerio de Ciencia e Innovación, Spain, (Project CTQ 2008-02200/BQU) and Junta de Castilla y León (Grupo de Excelencia GR-65) are gratefully acknowledged for financial support of this work. Diego García-Gómez gratefully acknowledges financial assistance from a Formación de Profesorado Universitario (FPU) grant of the Ministerio de Educación. The authors thank Dr. C. Raposo (Servicio General de Espectrometría de Masas, Universidad de Salamanca) for assessment and technical support.

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Authors and Affiliations

  1. Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Química, Universidad de Salamanca, 37008, Salamanca, Spain

    E. Rodríguez-Gonzalo, D. García-Gómez & R. Carabias-Martínez

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  1. E. Rodríguez-Gonzalo
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  2. D. García-Gómez
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  3. R. Carabias-Martínez
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Correspondence to E. Rodríguez-Gonzalo.

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Rodríguez-Gonzalo, E., García-Gómez, D. & Carabias-Martínez, R. A confirmatory method for the determination of phenolic endocrine disruptors in honey using restricted-access material–liquid chromatography–tandem mass spectrometry. Anal Bioanal Chem 398, 1239–1247 (2010). https://doi.org/10.1007/s00216-010-3621-z

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  • DOI: https://doi.org/10.1007/s00216-010-3621-z

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