Determination of tetracycline residues in soil by pressurized liquid extraction and liquid chromatography tandem mass spectrometry |
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Authors: | Vicente Andreu Pablo Vazquez-Roig Cristina Blasco Yolanda Picó |
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Institution: | (1) Centro de Investigaciones sobre Desertificación (CIDE), (CSIC, Universitat de València, Generalitat Valenciana), Camí de la Marjal s/n, 46470 Albal, Valencia, Spain;(2) Laboratori de Bromatologia, Facultat de Farmàcia, Universitat de València, Av, Vicent Andrés s/n, 46100 Burjassot, València, Spain |
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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.
Electronic supplementary material The online version of this article (doi: ) contains supplementary material, which is available to authorized users. |
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Keywords: | Antibacterials Tetracyclines LC-MS/MS Pressurized liquid extraction Environmental analysis Soil |
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