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Determination of tetracycline residues in soil by pressurized liquid extraction and liquid chromatography tandem mass spectrometry

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Abstract

An optimized extraction and cleanup method for the analysis of chlortetracycline (CTC), doxycycline (DC), oxytetracycline (OTC) and tetracycline (TC) in soil is presented. Soil extraction in a pressurized liquid extraction system, followed by extract clean up using solid-phase extraction (SPE) and tetracycline determination by liquid chromatography tandem mass spectrometry (LC-MS/MS) provided appropriate efficiency and reproducibility. Different dispersing agents and solvents for soil extraction and several SPE cartridges for cleanup were compared. The best extraction results were obtained using ethylenediamine tetraacetic acid-treated sand as dispersing agent, and water at 70 °C. The most effective cleanup was obtained using Strata-XTM sorbent in combination with a strong anion exchange cartridge. Recoveries ranged from 71% to 96% and precision, as indicated by the relative standard deviations, was within the range of 8–15%. The limits of quantification (LOQs) by using LC-MS/MS, based on signal-to-noise ratio (S/N) of 10, ranged from 1 μg kg−1 for TC to 5 μg kg−1 for CTC. These results pointed out that this technique is appropriate to determine tetracyclines in soils. Analysis of 100 samples taken in the Valencian Community revealed that, in soil, up to 5 μg kg−1 CTC, 15 μg kg−1 OTC, 18 μg kg−1 TC, and 12 μg kg−1 DC could be detected. Detection of the analytes in several samples, which typify great part of the Spanish agricultural soils, should be outlined as most important result of this study.

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Acknowledgments

The authors thank the Spanish Ministry of Science and Innovation together with the European Regional Development Funds (ERDF; projects GCL2007-66687-C02-01/BOS, CGL2007-66687-C02-02 and CGL2008-01693/BTE), the Conselleria d’Empresa, Universitat i Ciència through an R+D project for emerging research groups (GV/2007/264), and the Conselleria de Sanitat (project EVES2008-011) for financial support. P.V.R thanks the Spanish Ministry of Science and Innovation for the FPI grant.

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Authors and Affiliations

  1. Centro de Investigaciones sobre Desertificación (CIDE), (CSIC, Universitat de València, Generalitat Valenciana), Camí de la Marjal s/n, 46470, Albal, Valencia, Spain

    Vicente Andreu

  2. Laboratori de Bromatologia, Facultat de Farmàcia, Universitat de València, Av, Vicent Andrés s/n, 46100, Burjassot, València, Spain

    Pablo Vazquez-Roig, Cristina Blasco & Yolanda Picó

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  1. Vicente Andreu
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  2. Pablo Vazquez-Roig
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  3. Cristina Blasco
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  4. Yolanda Picó
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Corresponding author

Correspondence to Yolanda Picó.

Electronic Supplementary Material

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Table S1

Physico chemical characteristics of the soil samples (DOC 159 KB)

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Andreu, V., Vazquez-Roig, P., Blasco, C. et al. Determination of tetracycline residues in soil by pressurized liquid extraction and liquid chromatography tandem mass spectrometry. Anal Bioanal Chem 394, 1329–1339 (2009). https://doi.org/10.1007/s00216-009-2635-x

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  • DOI: https://doi.org/10.1007/s00216-009-2635-x

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