Abstract
Hybrid materials based on polystyrene (PS) and green metal-organic frameworks (MOFs) were synthesized, characterized, and evaluated as potential sorbents in dispersive micro-solid-phase extraction (µ-dSPE). Among the resulting materials, the hybrid PS/DUT-67(Zr) was selected as the adequate extraction material for the monitoring of six personal care products in micellar cosmetic samples, combining the µ-dSPE method with ultra-high performance liquid chromatography (UHPLC) coupled to ultraviolet/visible detection (UV/Vis). Univariate studies and a factorial design were performed in the optimization of the microextraction procedure. The compromise optimum extraction conditions included 20 mg of PS/DUT-67(Zr) for 10 mL of sample, 2 min of extraction time, and two desorption steps using 100 µL of acetonitrile and 5 min assisted by vortex in each one. The validated μ-dSPE-UHPLC-UV/Vis method presented limits of detection and quantification down to 3.00 and 10.0 μg·L−1, respectively. The inter-day precision values were lower than 23.5 and 21.2% for concentration levels of 75 μg·L−1 and 650 μg·L−1, respectively. The hydrophobicity of the resulting PS/DUT-67(Zr) material was crucial for the improvement of its extraction capacity in comparison with its unitary components, showing the advantages of combining MOFs with other materials, getting new sorbents with interesting properties.
Highlights
Sample preparation remains as a crucial step nowadays to ensure: (i) proper elimination of the interferences present in a sample, (ii) the preconcentration of target analytes present at trace levels in the sample, and (iii) the compatibility with the further analytical instruments [1], for complex samples and despite advances in analytical instrumentation
Optimization of the μ-dSPE Method. To evaluate if this hydrophobic hybrid PS/DUT-67(Zr) material is an interesting sorbent, valid to perform as an alternative to other sorbents for the monitoring of personal care products (PCPs) using a μ-dSPE-ultra-high performance liquid chromatography (UHPLC)-ultraviolet/visible detection (UV/Vis) method, different variables were considered in the optimization, such as the sorbent amount, the desorption solvent, and the extraction and desorption times
Novel hybrid materials based on PS and metal-organic frameworks (MOFs), such as DUT-67(Zr) and CIM-80(Al), were successfully synthesized by dispersion polymerization of styrene
Summary
Sample preparation remains as a crucial step nowadays to ensure: (i) proper elimination of the interferences present in a sample, (ii) the preconcentration of target analytes present at trace levels in the sample, and (iii) the compatibility with the further analytical instruments [1], for complex samples and despite advances in analytical instrumentation. Different MOF-based composites and hybrid materials have been reported by incorporating them into inorganic materials (mesoporous silica) [21,22], polymers [23,24], metal oxide particles [25,26], and carbonaceous materials such as graphene oxide, carbon nanotubes, etc., [25,27] This advance has made possible the design of sorbent materials with novel physicochemical features that lead to an enhancement of MOFs extraction performance by giving them higher structural support, by protecting their pores, or even by providing them with hydrophobicity and magnetic properties. Adequate aliquots of the samples were diluted up to 100 mL, and the pH value was measured
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