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Abstract
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In this study, an air-assisted liquid–liquid microextraction (AALLME) method has been developed for
simultaneous derivatization, extraction, and preconcentration of some phenolic pollutants in aqueous
samples before their determination by gas chromatography-flame ionization detection (GC-FID). In
order to improve the chromatographic behavior of phenolic compounds, the analytes were derivatized
with butyl chloroformate (BCF) and extracted simultaneously into 1,1,1-trichlorethane. The effects of
different parameters influencing the extraction efficiency including extraction solvent type and its
volume, ionic strength, volume of derivatization agent, and extraction numbers were investigated and
optimized for the simultaneous derivatization/microextraction procedure. Under the optimum extraction
conditions, the method showed wide linear ranges (LRs) between 1–2000 mg L1. The other analytical
parameters were obtained in the following ranges: enrichment factors (EFs) 2020–2761, enhancement
factors (EnFs) 2225–3807, extraction recoveries (ERs) 65–88%, and limits of detection (LODs) 0.1–0.4 mg
L1. Relative standard deviations (RSDs) for the extraction of 100 and 200 mg L1 of each selected phenol
(n ¼ 6) were obtained in the ranges of 2–4% and 1–4%, respectively. Finally, the target phenols were
determined in different samples such as tap water, river water, petrochemical wastewater, refinery
wastewater, and municipality wastewater by the proposed AALLME-GC-FID method
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