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Determination of tetracyclines in soils with pressurized liquid extraction and liquid chromatography-tandem mass spectrometry

AuthorsVázquez-Roig, Pablo; Andreu Pérez, V. ; Blasco, Cristina; Picó, Yolanda
Issue DateJan-2010
Citation11th International Symposium on Hyphenated Techniques in Chromatography and Hyphenated Chromatographic Analyzers (2010)
AbstractAn 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 A degrees C. The most effective cleanup was obtained using Strata-X-TM 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 mu g kg(-1) for TC to 5 mu g 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 mu g kg(-1) CTC, 15 mu g kg(-1) OTC, 18 mu g kg(-1) TC, and 12 mu g 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.
DescriptionPoster presentado en el 11th International Symposium on Hyphenated Techniques in Chromatography and Hyphenated Chromatographic Analyzers celebrado en Bruges (Bélgica) del 27 al 29 enero de 2010
Appears in Collections:(CIDE) Comunicaciones congresos
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