A novel sorbent for solid phase extraction (SPE) based on hybrid nanofibrous polycaprolactone containing graphene nanoparticles has been prepared. The preparation of hybrid polymer nanofibers with a very high 1:1 polymer/graphene ratio was achieved for the first time using alternating current electrospinning. The final appearance of these nanofibers was a thick porous layer that was cut into the shape of easy-to-handle extraction discs. Based on the preliminary study in which the graphene content varied, 30% graphene-doped nanofibers (w/w) exhibited the highest recoveries and enabled a significant increase in the retention of analytes, 2-25 times in comparison to PCL. The incorporation of graphene resulted in a higher surface area of 12 g/m2 compared to 2 g/m2 determined for the native polycaprolactone (PCL) nanofibers. This unique material was applied for a simple stirred disc sorptive extraction and preconcentration of trace levels of emerging organic environmental contaminants, bisphenols A, AF, AP, C, S, Z, 3-chlorophenol, and pesticides fenoxycarb, deltamethrin, and kadethrin from surface waters prior to HPLC-DAD determination. This was accomplished by stirring the unsupported nanofiber disc in a large-volume sample with RSD of five extractions of 3-15%. Recoveries yielded 87-120%, except 52% for bisphenol S due to its high polarity. Optimization of the extraction procedure included conditioning, sample volume, extraction time, and elution solvent. Our novel desorption procedure carried out in a vial used for the direct injection into the HPLC system significantly reduced sample handling and minimized potential human error.

Charles University Faculty of Pharmacy in Hradec Králové The Department of Analytical Chemistry Ak Heyrovského 1203 500 05 Hradec Králové Czech Republic

Technical University of Liberec Faculty of Textile Engineering Department of Nonwovens and Nanofibrous Materials Studentská 2 461 17 Liberec Czech Republic

Citace poskytuje Crossref.org