Synthesis and characterization of polyamide-graphene oxide-polypyrrole electrospun nanofibers for spin-column micro solid phase extraction of parabens in milk samples

摘要

In the present study, an electrospun composite of polyamide-graphene oxide-polypyrrole was synthesized. The characterization of the synthesized material was accomplished using field emission scanning electron microscopy (FESEM) and Fourier transform infrared spectroscopy (FT-IR). FESEM images showed uniform and beadles nanofibers. The composite was employed as a novel sorbent for spin-column micro solid phase extraction to determine parabens in milk samples. Addition of graphene oxide and polypyrrole into the polymeric network of polyamide significantly improves the extraction efficiency of the electrospun sorbent due to providing the possibility of various interactions with the target analytes such as hydrogen bonding, hydrophobic and pi-pi stacking. All effective parameters on the efficiency of both adsorption and desorption steps were optimized. These parameters were pH of sample solution (5.0), sorbent amount (20 mg), type and volume of desorption solvent (200 mu L of methanol), number of cycles (7 and 14) and centrifugation speed (600 and 500 rpm) of both adsorption and desorption steps. Under the optimal conditions, the calibration plots were linear within the range of 10-1000,15-1000, and 20-1000 ng mL(-1) for methyl paraben, ethyl paraben and propyl paraben, respectively. Limits of detection were obtained lower than 7.0 ng mL(-1) by HPLC-UV. Intra- and inter-assay relative standard deviations were less than 8.6% and 5.8%, respectively. Finally, the method was successfully applied for determination of parabens in some milk samples and good recoveries were obtained within the range of 81.7-97.8%. The results demonstrated good efficiency of the synthesized electrospun composite nanofibers as the packing material for spin-column micro solid phase extraction. (C) 2019 Elsevier B.V. All rights reserved.