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Determination of tetracyclines in milk samples by magnetic solid phase extraction flow injection analysis

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Abstract

A method is presented for magnetic solid phase extraction (MSPE) of tetracyclines in milk samples. The method involves the extraction and clean-up by silica based magnetic support dispersion on non-pretreated milk samples, followed by the magnetic isolation and desorption of the analytes by acidified methanol. The tetracyclines eluted from the magnetic support were determined simultaneously by flow injection analysis with spectrophotometric detection. Under optimal conditions, the linear range of the calibration curve ranges from 0.03 to 0.60 mg L−1, with a limit of detection of 10 μg L−1. Recoveries were determined for milk spiked at levels from 0.15 to 0.60 mg L−1. Average recoveries ranged from 91.0 to 97.0%, with a precision of <5.0% in all cases. The method was validated by comparing the results with those obtained by MSPE-HPLC and SPE-HPLC. No significant differences were observed (p < 0.05)

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Acknowledgments

The authors wish to thank the CONACyT (project 2006-61310), PROMEP (SIATA-Project), and Consellería de Economía e Industria proyecto INCITE09 261 380 PR for financial support.

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Authors and Affiliations

  1. Centro de Investigaciones Químicas, Universidad Autónoma del Estado de Hidalgo, Carr. Pachuca Tulancingo Km 4.5, 42076, Pachuca, Hgo, Mexico

    Jose A. Rodriguez, Johanan Espinosa, Karina Aguilar-Arteaga & Israel S. Ibarra

  2. Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Veterinaria, Universidad de Santiago de Compostela, 27002, Lugo, Spain

    Jose M. Miranda

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  1. Jose A. Rodriguez
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  2. Johanan Espinosa
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  3. Karina Aguilar-Arteaga
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  4. Israel S. Ibarra
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  5. Jose M. Miranda
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Correspondence to Jose A. Rodriguez.

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Rodriguez, J.A., Espinosa, J., Aguilar-Arteaga, K. et al. Determination of tetracyclines in milk samples by magnetic solid phase extraction flow injection analysis. Microchim Acta 171, 407–413 (2010). https://doi.org/10.1007/s00604-010-0428-8

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  • DOI: https://doi.org/10.1007/s00604-010-0428-8

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