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Published on: July 11, 2014
Ethylene glycol-based dispersive liquid-liquid microextraction of bisphenols in edible oil samples
Cristina Zapater1, Lorena Vidal1, Miguel Ángel Aguirre1
1Department of Analytical Chemistry, Nutrition and Food Science, University Institute of Materials, Faculty of Science, University of Alicante, P.O. Box 99, 03080, Alicante, Spain.
Abstract:
This study compares, for the firt time, the use of three different ethylene glycol-based extractant solvents in dispersive liquid-liquid microextraction (DLLME) for the determination of four bisphenols (i.e., BPF, BPA, BPAP, and BPAF) in edible oils by liquid chromatography-diode array detector (LC-DAD). The extractants studied were: pure ethylene glycol (EG), a deep eutectic solvent or DES (i.e., chlorine chloride (ChCl) and EG, 1:2 M ratio), and a magnetic deep eutectic solvent or MDES (i.e., ChCl, EG and iron chloride hexahydrate (FeCl3·6H2O), 1:4:1 M ratio). Two-step multivariate optimization was performed for EG and DES, while one-step optimization was applied for MDES. The optimal conditions for EG and DES were similar with 50 μL of extractant volume and 1 min of extraction time, except for centrifugation conditions which were 3 min and 370 g-force and 3 min and 832 g-force for EG and DES, respectively. The use of MDES required a higher volume of extractant (i.e., 75 μL) and a longer extraction time (i.e., 4.5 min). The most satisfactory results were achieved using EG, exhibiting adequate linearity (r ≥ 0.990), lower limits of detection (LODs) (i.e., 0.3 μg kg-1), excellent repeatability (RSD ≤3.2 %) for all analytes and non-significant matrix effects in real edible oil samples (i.e., relative recovery values: 71-121 %). Therefore, pure ethylene glycol is the most suitable extractant when compared to ethylene glycol-based eutectic mixtures and their magnetic variant. This finding underscores the necessity for further exploration of the pure constituents of mixtures as potential extractants.

