The use of solid-phase microextraction coatings based on gold nanoparticles was investigated, focusing the attention on the preparation of nanoparticles with nonclassical reduction agents of HAuCl such as gallic acid and H O , rather than the conventional sodium citrate. All nanoparticles were characterized by diode array spectroscopy, whereas novel nanoparticles prepared with gallic acid and H O were also characterized by microscopic techniques. Solid-phase microextraction coatings were prepared with a layer-by-layer approach. Gallic acid permitted the preparation of stable nanoparticles with milder experimental conditions (1 min, room temperature) and provided the most uniform coatings (thickness ∼3 μm). Seven organochlorine pesticides were determined in different environmental waters using gas chromatography with electron capture detection. Despite the low thickness of the coatings, limits of detection of the entire method down to 0.13 μg/L were obtained. A comparison with the commercial polyacrylate in terms of the partition coefficients of the analytes to the coatings gave logarithm of the partition coefficient values two times higher with gallic acid than polyacrylate (although the commercial fiber is 28 times thicker). Interfiber relative standard deviation values ranged from 8.67 to 21.3%. Optimum fibers also presented an adequate lifetime (>100 extractions).
The authors describe a new coating for use in solid-phase microextraction (SPME). Silver nanoparticles (AgNPs) were prepared by using gallic acid or glucose as the reducing agents, and then supported onto a stainless steel wire that was previously coated with a silver mirror. Coating with AgNPs was performed by a layer-by-layer approach of up to eight cycles of consecutive deposition of AgNPs and the thiol linker 1,8-octanedithiol. This procedure allows proper control of the coating thickness. Thicknesses are 3.2 μm and 3.5 μm with AgNPs obtained with gallic acid and glucose, respectively. This is in agreement with theoretical estimations (3.8 μm). The fibers were used in the direct-immersion SPME-GC-FID determination of 16 polycyclic aromatic hydrocarbons (PAHs) from different waters. The performance of the method was compared to the one using polydimethylsiloxane fibers (100 μm), which is the most suitable commercial SPME fiber for PAHs. Despite the low thickness of the AgNP coatings (compared to PDMS), the analytical features of the method using the most adequate coating (AgNPs prepared with gallic acid) include: (a) limits of detection down to 0.6 ng·mL; (b) intra-day, inter-day, and inter-fiber precisions (expressed as RSDs) lower than 22, 26 and 25%, respectively; and (c) an operational lifetime of ~150 extractions/desorption cycles. The analysis of various spiked environmental waters using these fibers resulted in adequate analytical performance. Graphical abstract Silver nanoparticle based coatings for solid-phase microextraction fibers were prepared by a layer-by-layer approach. They were used for determination of 16 PAHs in waters by gas chromatography. Limits of detection are < 14 μg·L and intra-day, inter-day, and inter-fiber precisions are <26%.
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.
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