Trace Analysis of Phenols and Chlorophenols in Water by in Situ Derivatization Headspace Solid-Phase Microextraction Coupled with Gas Chromatography/Mass Spectrometry

An in situ derivatization headspace solid phase microextraction method has been developed for the determination of phenols and related chlorophenols in water.Acetylated derivatives were selectively determined using gas chromatography/mass spectrometry(GC /MS).Parameters affecting both derivatization and SPME procedures,such as fiber coating,extraction time,temperature,volume of derivatizating reagent and ionic strength,were studied.Then the polydimethylsiloxane/divinylbenzene fiber(PDMS/DVB,65 μm) was selected.The performance of the method was evaluated in terms of accuracy,linearity,precision and limits of detection.Under the selected conditions,i.e.4.0 g NaCl,0.10 g Na2HPO4 in every 10 mL sample solution,headspace extraction at 60℃ and 600 r/min for 30 min,quantitative recoveries and satisfactory precision(RSD≤13.7%) were obtained.Limits of detection for all target compounds ranged from 0.014 to 0.044 μg/L.Linearity was found in a wide range of concentrations.Finally,the applicability of the proposed method is demonstrated by determining phenols in real wastewater samples.