PMID- 25770896 OWN - NLM STAT- MEDLINE DCOM- 20150721 LR - 20181202 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1391 DP - 2015 Apr 24 TI - Determination of estrogenic mycotoxins in environmental water samples by low-toxicity dispersive liquid-liquid microextraction and liquid chromatography-tandem mass spectrometry. PG - 1-8 LID - S0021-9673(15)00340-4 [pii] LID - 10.1016/j.chroma.2015.02.067 [doi] AB - 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, alpha-zearalanol, beta-zearalanol, alpha-zearalenol and beta-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 muL 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 beta-zearalanol and zearalanone in the river water samples. CI - Copyright (c) 2015 Elsevier B.V. All rights reserved. FAU - Emidio, Elissandro Soares AU - Emidio ES AD - Analytical Chemistry Department, Chemistry Institute, Sao Paulo State University-UNESP, Araraquara, SP 14801-970, Brazil. FAU - da Silva, Claudia Pereira AU - da Silva CP AD - Analytical Chemistry Department, Chemistry Institute, Sao Paulo State University-UNESP, Araraquara, SP 14801-970, Brazil. FAU - de Marchi, Mary Rosa Rodrigues AU - de Marchi MR AD - Analytical Chemistry Department, Chemistry Institute, Sao Paulo State University-UNESP, Araraquara, SP 14801-970, Brazil. Electronic address: mssqam@iq.unesp.br. LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20150301 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Estrogens, Non-Steroidal) RN - 0 (Mycotoxins) RN - 0 (zearalenol) RN - 5W827M159J (Zearalenone) RN - 76LO2L2V39 (Zeranol) RN - HUN219N434 (taleranol) SB - IM MH - Chromatography, Liquid/methods MH - Estrogens, Non-Steroidal/*analysis MH - Fresh Water/chemistry MH - Limit of Detection MH - Liquid Phase Microextraction MH - Mycotoxins/*analysis MH - Spectrometry, Mass, Electrospray Ionization/methods MH - Tandem Mass Spectrometry/methods MH - Zearalenone/*analysis MH - Zeranol/*analogs & derivatives/*analysis OTO - NOTNLM OT - Bromosolvents OT - Dispersive liquid-liquid microextraction OT - Estrogenic mycotoxins OT - LC-MS/MS OT - Water samples EDAT- 2015/03/17 06:00 MHDA- 2015/07/22 06:00 CRDT- 2015/03/16 06:00 PHST- 2014/10/29 00:00 [received] PHST- 2015/02/18 00:00 [revised] PHST- 2015/02/23 00:00 [accepted] PHST- 2015/03/16 06:00 [entrez] PHST- 2015/03/17 06:00 [pubmed] PHST- 2015/07/22 06:00 [medline] AID - S0021-9673(15)00340-4 [pii] AID - 10.1016/j.chroma.2015.02.067 [doi] PST - ppublish SO - J Chromatogr A. 2015 Apr 24;1391:1-8. doi: 10.1016/j.chroma.2015.02.067. Epub 2015 Mar 1.