A novel hybrid mesostructured silica for the solid-phase extraction of estrogenic hormones from waters

Abstract

Mesoporous silica functionalized with octadecyl groups (denoted as SBA-15-C 18 ) was prepared and characterized. The adsorption capacity of the prepared SBA-15-C 18 for a mixture of twelve endocrine disrupting compounds (synthetic and natural estrogenic hormones) in aqueous media was evaluated by off-line solid-phase extraction (SPE) and compared with a commercial phase for SPE (ExtraBond® C 18 ). Analytes were determined by high performance liquid chromatography with UV-vis detection. Under optimized conditions (100 mg of SBA-15-C 18 sorbent; conditioning: 2 mL methanol and 2 mL Milli-Q water; loading: 150 mL water sample; washing: 5 mL Milli-Q water; elution: 2 mL methanol; flow rate 0.5 mL min À1 ) the preconcentration factor achieved was 1000. The analytical characteristics of this methodology were evaluated, showing good precision, accuracy and linearity, with method quantification limits (MQLs) between 0.16 and 3.00 mg L À1 . The SBA-15-C 18 material enabled the extraction of the twelve estrogenic hormones in tap water (pH 6.6), mineral water (pH 5.0), groundwater (pH 7.3), river water (pH 5.0) and effluent wastewater (pH 5.0) with recoveries between 70 and 112% at the lower level studied (MQL). Fig. 3 Comparison of the recovery percentages obtained from the analysis (n ¼ 3) of 50 mL sample volume of spiked Milli-Q water at 450 mg L À1 extracted with SPE cartridges packed with commercial silica (ExtraBond® C 18 ) and mesoporous silica ). This journal is

Evaluation of mesostructured silica materials with different structures and morphologies as carriers for quercetin and naringin encapsulation

“…Moreover, the stability of mesostructured silicas has also been checked when a functionalization on the material has been done (which is not the case). For instance, even when large ligands like C18 (octadecylsilane) groups have been attached, changes in the structure of the pore size distribution have never been detected in the modified materials [63].…”

Current development and applications of ordered mesoporous silicas and other sol–gel silica-based materials in food sample preparation for xenobiotics analysis

“…To assess the potential of OMSs as sorbents in food sample preparation, different studies have been carried out in the last years for SPE [34][35][36][37][38][39][40][41], µ-SPE [41] and MSPD [42,43] applications (Table 1). In most of these works, results have been compared with those obtained with commercial products, in terms of sensitivity and selectivity, demonstrating their promising application for this purpose.…”

“…Results obtained indicated that the prepared mesoporous sorbent enabled the extraction of the twelve estrogenic hormones in tap and mineral waters with recoveries between 70 and 111% (RSD ≤ 10%) for the lowest concentration level tested. A preconcentration factor of 1000 was achieved under optimized conditions, and three loading and elution cycles could be applied without a significant decrease in the adsorption capacity [35].…”

One-pot synthesized functionalized mesoporous silica as a reversed-phase sorbent for solid-phase extraction of endocrine disrupting compounds in milks

“…The mixture was vortexed during 2 min and after was centrifuged at 4000 rpm for 5 min to separate the precipitate. Finally, the 14 supernatant was decanted and diluted with water to a final volume of 25 mL (to reduce the MeOH to 10, 15 or 20% by volume, respectively) and, then, the extract was purified by SPE according to the protocol described in previous works [16,23]. Results obtained indicated that the use of a lower volume of MeOH provides higher recoveries for E3, PRED, NAN, 17β-E2 and T, with an important increase of 60% in the recovery of E3 and of 50% in the recovery of PRED.…”