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Ultrasensitive, simple and solvent-free micro-assay for determining sulphite preservatives (E220–228) in foods by HS-SDME and UV–vis micro-spectrophotometry

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Abstract

A new method based on headspace single-drop microextraction in combination with UV–vis micro-spectrophotometry has been developed for the ultrasensitive determination of banned sulphite preservatives (E220–228) in fruits and vegetables. Sample acidification was used for SO2 generation, which is collected onto a 5,5′-dithiobis-(2-nitrobenzoic acid) microdrop for spectrophotometric measurement. A careful study of this reaction was necessary, including conditions for SO2 generation from different sulphating salts, drop pH, 5,5′-dithiobis-(2-nitrobenzoic acid) concentration and potential interference effects. Variables influencing mass transfer (stirring, sample volume and addition of salt) and microextraction time were also studied. A simple sulphite extraction was carried out, and problems caused by oxidation during the extraction process were addressed. A high enrichment factor (380) allows the determination of low levels of free SO2 in fruits and vegetables (limit of detection 0.06 μg g−1, limit of quantification 0.2 μg g−1) with an adequate precision (repeatability, relative standard deviation 5 %). In addition, the sulphiting process was studied through the monitoring of residual SO2 in a vegetal sample, thus showing the importance of a sensitive tool for SO2 detection at low levels.

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Acknowledgments

Financial support from the Spanish Ministry of Science and Innovation (project CTQ2012-32788) and the Xunta de Galicia (project 10PXIB 314030 PR) is gratefully acknowledged.

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Authors and Affiliations

  1. Departamento de Química Analítica y Alimentaria, Área de Química Analítica, Facultad de Química, Universidad de Vigo, Campus As Lagoas-Marcosende s/n, 36310, Vigo, Spain

    E. Gómez-Otero, M. Costas, I. Lavilla & C. Bendicho

Authors
  1. E. Gómez-Otero
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  2. M. Costas
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  3. I. Lavilla
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  4. C. Bendicho
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Corresponding author

Correspondence to C. Bendicho.

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Published in the topical collection Microextraction Techniques with guest editors Miguel Valcárcel Cases, Soledad Cárdenas Aranzana and Rafael Lucena Rodríguez.

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Gómez-Otero, E., Costas, M., Lavilla, I. et al. Ultrasensitive, simple and solvent-free micro-assay for determining sulphite preservatives (E220–228) in foods by HS-SDME and UV–vis micro-spectrophotometry. Anal Bioanal Chem 406, 2133–2140 (2014). https://doi.org/10.1007/s00216-013-7293-3

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  • DOI: https://doi.org/10.1007/s00216-013-7293-3

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