Development, validation and application of an HPLC method for phenol electrooxidation products in the presence of chloride

Abstract

<div><p>A high-performance liquid chromatography (HPLC) method was developed and validated to determine phenol and potential intermediates from hydroxylation (hydroquinone, benzoquinone, catechol) and hypochlorination (2-chlorophenol, 3-chlorophenol, 4-chlorophenol, 2,4-dichlorophenol, 2,6-dichlorophenol, 2,3,6-trichlorophenol, 2,4,5-trichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol) pathways during electrooxidation in the presence of chloride. A Hypersil ODS column (150 mm L × 4.6 mm I.D.) was used for the separation. The best separation was achieved when using a time variant gradient between a water mobile phase (with 0.1% formic acid adjusted to pH 3.0 with 0.1 mM sulfuric acid) and an organic phase (90:5:5 by volume mixture of acetonitrile:methanol:acetic acid). The flow rate was 0.8 mL min⁻¹ and UV absorbance was monitored at 270, 280, 290 and 300 nm, choosing the wavelength of strongest response for each compound. The intra- and inter-day accuracy and precision were tested using five replicates each day on three consecutive days.</p></div