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Determination of estrogens in environmental water samples using 1,3‐dipentylimidazolium hexafluorophosphate ionic liquid as extraction solvent in dispersive liquid–liquid microextraction
Author(s) -
SocasRodríguez Bárbara,
HernándezBorges Javier,
AsensioRamos María,
HerreraHerrera Antonio V.,
Palenzuela Jose A.,
RodríguezDelgado Miguel Ángel
Publication year - 2014
Publication title -
electrophoresis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.666
H-Index - 158
eISSN - 1522-2683
pISSN - 0173-0835
DOI - 10.1002/elps.201400024
Subject(s) - hexafluorophosphate , chromatography , ionic liquid , chemistry , extraction (chemistry) , solvent , disperser , high performance liquid chromatography , detection limit , analytical chemistry (journal) , materials science , organic chemistry , composite material , catalysis
In this work, the potential of a symmetric dialkyl‐substituted ionic liquid ( IL ), 1,3‐dipenthylimidazolium hexafluorophosphate ([ PPI m][ PF 6 ]), as extraction solvent in dispersive liquid–liquid microextraction ( DLLME ) has been studied for the analysis of a group of three natural (estriol, 17β‐estradiol, and 17α‐estradiol) and four synthetic (17α‐ethynylestradiol, diethylstibestrol, dienestrol, and hexestrol) estrogenic compounds as well as one mycotoxin with estrogenic activity (zearalenone) in different types of water samples (Milli‐Q, mineral, and wastewater). Separation, determination, and quantification were developed by HPLC ‐ DAD and a fluorescence detector ( FD ) connected in series. Factors influencing the IL ‐ DLLME procedure (sample pH, amount of IL , type and volume of disperser solvent, ionic strength, and assistance of vortex agitation) were investigated and optimized by means of a step‐by‐step approach. Once the optimum extraction conditions were established (10 mL of water at pH 8, 60 mg of [ PPI m][ PF 6 ], 500 μL of ACN as disperser solvent and vortex agitation for 1 min), the calibration curves of the whole method ( IL ‐ DLLME ‐ HPLC ‐ DAD / FD ) were obtained and precision and accuracy were evaluated. It was demonstrated that the developed methodology was repeatable, accurate, and selective with limits of detection in the 0.30–0.57 μg/L and 13.8–37.1 μg/L range for FD and DAD , respectively. Relative recovery values were higher than 85% for the different types of water samples and the S tudent's t test demonstrated that there were not significant differences between the added and the found concentration.