Abstract
A novel coating based on hybrid monolith with metal–organic framework (MOF) onto conventional Teflon-coated magnetic stir bars was developed. For this purpose, the external surface of the Teflon stir bar was firstly vinylized in order to immobilize a glycidyl methacrylate (GMA)–based polymer onto the magnet. Then, an amino-modified MOF of type MIL-101 (NH2-MIL-101(Al)) was covalently attached to the GMA-based monolith. After the synthesis process, several parameters affecting extraction of target estrogens by stir bar sorptive extraction (SBSE) including pH, ionic strength, extraction time, stirring rate, desorption solvent, and desorption time were also investigated. The resulting hybrid monolith was evaluated as SBSE sorbent for extraction of three estrogens (estrone, 17β-estradiol, estriol) and synthetic 17β-ethinylestradiol from water and human urine samples followed by HPLC with fluorescence detection (excitation and emission wavelengths, 280 and 310 nm, respectively). Under the optimal experimental conditions, the analytical figures of the method were established, achieving satisfactory limits of detection in the range of 0.015–0.58 µg L−1, recovery results ranging from 70 to 95% with RSD less than 6%, and precision values (intra- and inter-extraction units) below 6%.Graphical abstract
Highlights
Estrogens are known as endocrine-disruptor compounds (EDCs) widely spread in the aquatic system and other environments
Several water-stable aminomodified metal–organic framework (MOF) based on MIL-101 type were selected taking into account the following characteristics: (i) the presence of amino groups in their structure allows that these materials can be attached covalently to the epoxide moieties onto the glycidyl methacrylate (GMA) monomers through nucleophilic substitution reactions [31]; (ii) the adequate MIL-101 typology in terms of pore-cage structure to host the target compounds (Fig. S1); (iii) several interaction forces between these materials and analytes such as hydrophobic effects and π-π interaction and hydrogen bonding, among others
The first example of polymer monolith modified with MOF onto commercial PTFE magnets for stir bar sorptive extraction (SBSE) purposes is presented
Summary
Estrogens are known as endocrine-disruptor compounds (EDCs) widely spread in the aquatic system and other environments. The attendance- and endocrine-disrupting potency of these molecules in waters, soil, and food are 10,000 times higher than common synthetic chemicals, for example pesticides [1,2,3]. Estrone (E1), 17β-estradiol (E2), 17β-ethinylestradiol (EE2), and estriol (E3) are the most extended estrogens in the environment and their origin can be various (human urine and feces, cattle activities, aquaculture, among others) [4]. These target analytes have been detected in environmental and wastewater samples [5,6,7].
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