Carbonized silk fibers for in-tube solid-phase microextraction to detect polycyclic aromatic hydrocarbons in water...

Silk fibers were carbonized to develop a biomass carbon material as an adsorbent for solid-phase microextraction. The surface structure of the carbonized silk fibers was characterized by scanning electron microscopy, and the graphitization degree was determined by Raman spectrometry. After carbonization under high temperature, the orderliness and structural regularity of carbon atoms on silk fibers were promoted. Extraction tube packed with carbonized silk fibers was prepared for in-tube solid-phase microextraction. Coupled with high performance liquid chromatography, it exhibited good extraction performance for hydrophobic polycyclic aromatic hydrocarbons. Main parameters including sampling volume, sampling rate, methanol content in sample, and desorption time were systematically investigated. Under the optimum conditions, the analysis method was established and it exhibited wide linear range (0.016-20 μg/L) with good linearity (correlation coefficient ≥ 0.9947), low limits of detection (0.005-0.050 μg/L), and high enrichment factors (1189-2775). Relative standard deviations (n = 3) for intraday (≤3.3%) and interday (≤9.6%) tests indicated that the extraction material had satisfactory repeatability. Finally, the analytical method was successfully applied to detect trace polycyclic aromatic hydrocarbons in real water samples, demonstrating its satisfactory practicability.