Three different approaches has been used to obtain nano/micro fibers and their diversity and extraction properties were examined. The effect of their structure on stability in an ultra-high-performance liquid chromatography (UHPLC) system during on-line SPE procedure was monitored. Five types of various nano/micro fiber polymers were used as sorbents: polyamide 6 nanofibers, polyvinylidene difluoride nanofibers, polyethylene microfibers, and two new polycaprolactone microfiber/nanofiber and polycaprolactone microfibers/polyvinylidene difluoride nanofibers composite polymers. The fiber polymers were filled in a cartridge directly connected to the UHPLC system and tested. For each polymer, the optimal conditions of the on-line extraction were found and potential applicability on real samples was tested. The determination of ochratoxin A (OTA) in beer matrix was chosen as a case study. Relevant factors such as the mechanical and chemical stability of the nano/microfibers, filling the cartridges, fiber reusability and the possibility and the repeatability of all processes were involved in the proposed study. A new nano/micro composite sorbent consisting of polycaprolactone microfibers/polyvinylidene difluoride nanofibers was chosen as the most suitable sorbent for the on-line extraction of OTA from a beer matrix. The tested validation parameters had the value of intra-day precision lower than 1.48%, linearity in the range from 0.5 to 100 μg L-1 with r2 ≥ 0.9999 for standard and matrix calibration curve, and recovery in the range 99.1-103.9% at five concentration levels. Long-term precision evaluated for 31 analyses over the period of three months did not exceed 2.9% RSD. It confirmed the column reusability and perfect stability of nano/micro composite sorbent in the presence of organic solvents and after repeated injection of a complex beer matrix.

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

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

The Technical University of Liberec The Institute for Nanomaterials Advanced Technology and Innovation Studentská 1402 2 46001 Liberec Czech Republic

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