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J Chromatogr A ; 1391: 1-8, 2015 Apr 24.
Artículo en Inglés | MEDLINE | ID: mdl-25770896

RESUMEN

A novel, simple, rapid and eco-friendly method based on dispersive liquid-liquid microextraction using a bromosolvent was developed to determine six estrogenic mycotoxins (zearalenone, zearalanone, α-zearalanol, ß-zearalanol, α-zearalenol and ß-zearalenol) in water samples by liquid chromatography-electrospray ionization tandem mass spectrometry in the negative mode (LC-ESI-MS/MS). The optimal conditions for this method include the use of 100 µL bromocyclohexane as an extraction solvent (using a non-dispersion solvent), 10 mL of aqueous sample (adjusted to pH 4), a vortex extraction time of 2 min, centrifugation for 10 min at 3500 rpm and no ionic strength adjustment. The calibration function was linear and was verified by applying the Mandel fitting test with a 95% confidence level. No matrix effect was observed. According to the relative standard deviations (RSDs), the precision was better than 13% for the repeatability and intermediate precision. The average recoveries of the spiked compounds ranged from 81 to 118%. The method limits of detection (LOD) and quantification (LOQ) considering a 125-fold pre-concentration step were 4-20 and 8-40 ng L(-1), respectively. Next, the method was applied to the analysis of the environmental aqueous samples, demonstrating the presence of ß-zearalanol and zearalanone in the river water samples.


Asunto(s)
Estrógenos no Esteroides/análisis , Micotoxinas/análisis , Zearalenona/análisis , Zeranol/análogos & derivados , Zeranol/análisis , Cromatografía Liquida/métodos , Agua Dulce/química , Límite de Detección , Microextracción en Fase Líquida , Espectrometría de Masa por Ionización de Electrospray/métodos , Espectrometría de Masas en Tándem/métodos
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