Abstract
A new technique for preparation of an unbreakable solid‐phase microextraction (SPME) fiber, using sol–gel technology is developed. Primarily, an ultrathin two‐dimensional intermediate film was prepared by hydrolysis of 3‐(trimethoxysilyl)‐1‐propanthiol self‐assembled monolayer grafted onto gold, then a stationary phase by electrodeposition of 3‐(trimethoxysilyl)propylmethacrylate as a precursor, tetramethyl orthosilicate and polyethylene glycol as a coating polymer was produced. The scanning electron microscopy images revealed that the new fiber exhibits a rather porous and homogenous surface. The thermal stability of the fabricated fiber was investigated by thermogravimetric analysis. The applicability of the prepared fiber coating in conjunction with gas chromatography‐mass spectrometry was examined by SPME of polycyclic aromatic hydrocarbons, as model analytes, from aquatic media. An extraction time of 20 min at 50°C gave maximum peak areas when NaCl, 15% was added to the aqueous samples. Limits of detection were in the range of 0.01–0.02 ng/mL and relative standard deviation values were in the range of 4–16% at 1 ng/mL. The developed method was successfully applied for the analysis of real water samples while the relative recovery percentage was in the range of 102–118%.