Full automatic determination of chlorophenols in water using solid-phase microextraction/on-fiber derivatization and gas chromatography-mass spectrometry

A fully automated combination of solid-phase microextraction and on-fiber derivatization coupled with gas chromatography-mass spectrometry was developed to determine 17 chlorophenols in aqueous samples. Optimal parameters for the automated process, such as fiber coating (polyacrylate), derivatization reagent (N,O-bis(trimethylsilyl) trifluoroacetamide), extraction time (60 min), derivatization time (5 min), incubation temperature (35 degrees C), sample pH (3), and ionic strength (300 g L-1 of NaCl), as well as desorption time (5 min) and desorption temperature (270 degrees C) were established. The whole procedure took only 90 min and was performed automatically. The shortcomings of silylation derivatives, like incompleteness and instability, were overcome by using solid-phase microextraction on-fiber silylation in this study. The results from both pure water and river water samples showed that the method had a good linearity (r2 = 0.99931.0000), ranging from 0.01 to 100 mu g L-1. The related standard deviations were between 3.6 and 10.0%. The limits of detections and qualifications ranged from 0.03 to 3.11 ng L-1 and 0.09 to 10.4 ng L-1 for the CPs, respectively. The proposed method is superior to traditional solid phase extraction procedure.