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A new extraction phase based on hydrogel disks of polyvinyl alcohol (PVOH) and pectin was proposed, characterized and evaluated for the extraction of six steroidal hormones (estriol, estrone, 17β-estradiol, 17α-ethinylestradiol, progesterone, and testosterone) in aqueous samples with subsequent determination by gas chromatography-tandem mass spectrometry (GC-MS/MS) after the derivatization procedure. The developed extraction procedure was based on the solid phase extraction (SPE) technique, but employed hydrogel as the sorbent phase. The effects of several parameters, including the amount and composition of the sorbent phase, pH, sample volume, flow rate, and gel swelling over the extraction efficiency, were evaluated. Gels with lower swelling indexes and larger amounts of sorbent ensured higher extraction yields of analytes. The main benefits of using the PVOH/pectin-based hydrogel as the extraction phase are the ease of synthesis, low-cost preparation, and the possibility of reusing the extraction disks. Limits of quantification of 0.5 μg L−1 for estrone and 17β-estradiol, and 1 μg L−1 for testosterone, 17α-ethinylestradiol, progesterone, and estriol were obtained. Accuracy values ranged from 80% to 110%, while the inter-assay precision ranged from 0.23% to 22.2% and the intra-assay from 0.55% to 12.3%. Since the sorbent phase has an amphiphilic character, the use of hydrogels is promising for the extraction of medium-to-high polarity compounds.

A novel alginate based hydrogel was successfully prepared and tested for the solid phase microextraction of medium-to-high polarity compounds, when supported in a polypropylene (PP) fiber. Pure alginate when added onto the surface of the PP fiber, resulted in a significant improvement in the extraction efficiency of the analytes (except for β-estradiol). The alginate hydrogel was modified upon the incorporation of a small amount of zein, a corn protein. Interestingly, the alginate/zein-supported hydrogel was capable of successfully extracting compounds with low partition constant (Kow), such as 17-α-ethinyl estradiol, progesterone and estriol, since the initial water uptake decreased dramatically in this gel, therefore, leaving the alginate hydroxyl groups more available to interact with the polar compounds. In conclusion, this paper presents the preparation of a simple, low cost, reusable, and efficient sorption phase for the extraction of polar compounds with different polarities in aqueous samples, which is a current technological challenge in developing efficient wastewater treatment.

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