Determination of estrogenic mycotoxins in environmental water samples by low-toxicity dispersive liquid-liquid microextraction and liquid chromatography-tandem mass spectrometry.

Autor: Emídio ES; Analytical Chemistry Department, Chemistry Institute, São Paulo State University-UNESP, Araraquara, SP 14801-970, Brazil., da Silva CP; Analytical Chemistry Department, Chemistry Institute, São Paulo State University-UNESP, Araraquara, SP 14801-970, Brazil., de Marchi MR; Analytical Chemistry Department, Chemistry Institute, São Paulo State University-UNESP, Araraquara, SP 14801-970, Brazil. Electronic address: mssqam@iq.unesp.br.
Jazyk: angličtina
Zdroj: Journal of chromatography. A [J Chromatogr A] 2015 Apr 24; Vol. 1391, pp. 1-8. Date of Electronic Publication: 2015 Mar 01.
DOI: 10.1016/j.chroma.2015.02.067
Abstrakt: 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, β-zearalanol, α-zearalenol and β-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 β-zearalanol and zearalanone in the river water samples.
(Copyright © 2015 Elsevier B.V. All rights reserved.)
Databáze: MEDLINE
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