Polymeric nano- and microfibers were tested as potential sorbents for the extraction of five neonicotinoids from natural waters. Nanofibrous mats were prepared from polycaprolactone, polyvinylidene fluoride, polystyrene, polyamide 6, polyacrylonitrile, and polyimide, as well as microfibers of polyethylene, a polycaprolactone nano- and microfiber conjugate, and polycaprolactone microfibers combined with polyvinylidene fluoride nanofibers. Polyimide nanofibers were selected as the most suitable sorbent for these analytes and the matrix. A Lab-In-Syringe system enabled automated preconcentration via online SPE of large sample volumes at low pressure with analyte separation by HPLC. Several mat layers were housed in a solvent filter holder integrated into the injection loop of an HPLC system. After loading 2 mL sample on the sorbent, the mobile phase eluted the retained analytes onto the chromatographic column. Extraction efficiencies of 68.8-83.4% were achieved. Large preconcentration factors ranging from 70 to 82 allowed reaching LOD and LOQ values of 0.4 to 1.7 and 1.2 to 5.5 µg·L-1, respectively. Analyte recoveries from spiked river waters ranged from 53.8% to 113.3% at the 5 µg·L-1 level and from 62.8% to 119.8% at the 20 µg·L-1 level. The developed methodology proved suitable for the determination of thiamethoxam, clothianidin, imidacloprid, and thiacloprid, whereas matrix peak overlapping inhibited quantification of acetamiprid.

• Keywords
• Lab-In-Syringe, membrane preconcentration, nanofibers, neonicotinoids, online SPE,
• Publication type
• Journal Article MeSH

This research involved the production of polycaprolactone fiber layers via the alternating current electrospinning method. To construct the micro/nanofiber scaffold, mixtures of two molecular weight solutions, M n 45 000 and M n 80 000, were spun in differing proportions in a solvent system containing acetic acid, formic acid, and acetone in a ratio of 1:1:1. The composite fiber materials with hydroxyapatite particles were prepared from a solution that combined the different molecular weight solutions at a ratio of 1:3. The study resulted in the preparation of fiber layers containing 0, 5, 10, and 15% (wt) hydroxyapatite particles from the dry mass of the polycaprolactone. The strength, wettability, and surface energy of the composite materials were examined, and the results demonstrated that hydroxyapatite affects the fiber diameters, strength, and surface energy and, thus, the wettability of the fiber layers. The fibrous layers produced were further tested for cytotoxicity and cell viability and proliferation. The results obtained thus strongly indicate that the resulting bulky micro/nanofiber layers are suitable for further testing with a view to their eventual application in the field of bone tissue engineering.

• Publication type
• Journal Article MeSH