Preconcentration of polar phenolic compounds from water samples and soil extract by liquid-phase microextraction and determination via liquid chromatography with ultraviolet detection.

This work proposes a liquid-phase microextraction (LPME) method to extract the highly polar compounds phenol (Ph), o-cresol (o-Cr), m-cresol (m-Cr), p-cresol (p-Cr), and 2,4-dimethylphenol (2,4-DMP) from aqueous matrices. The first extraction step of the LPME method employed a common volumetric flask and n-octanol, and the second extraction step used NaOH as the acceptor phase. The optimized extraction conditions were 900 µL of n-octanol as the extraction solvent, NaOH at 0.60 mol L(-1) as the acceptor phase, an extraction time of 5.0 min, HCl at 0.01 mol L(-1) and NaCl at 20.0% as the donor phase, and an extraction temperature of 20.0°C. The analysis of 50.0 mL of aqueous sample, pretreated under the optimized LPME conditions, afforded a limit of detection (LOD) between 0.3 and 3.5 µg L(-1), a limit of quantification (LOQ) between 1.2 and 11.6 µg L(-1), and a linear range from 2.50 to 50.0 µg L(-1) for Ph, o-Cr, m-Cr and p-Cr and from 12.5 to 250 µg L(-1) for 2,4-DMP. The proposed LPME method was a successful sample preparation strategy, and allowed for precise and accurate quantification of polar phenolic compounds in aqueous matrices such as tap water, river water, groundwater, and seawater, and also in a soil extract. The recovery values ranged from 72.5% to 126.0%, and the relative standard deviation was between 0.3 and 11.5%.

Interaction of phenol, o-cresol, and p-cresol with a clay-rich soil sample.

The present paper describes an interaction study of phenol, o-cresol, and p-cresol with a rich-clay soil sample (clay content of 62.3%). Experiments performed using long contact times, in concentrations of 50.0 mg L(-1) showed practically no signal of phenol, o-cresol, and p-cresol after 48, 72, and 120 h, respectively, suggesting a sorption process. Sorption experiments in the period of 24 h were carried out with the phenolic compounds in concentrations between 5.00 and 500.0 mg L(-1), and negligible interaction between the phenolic species and the soil was observed. Additional experiments were carried out using HgCl(2) or NaN(3) solution as biodegradation inhibitors. After 10 days of contact time in the presence of inhibitors, no alterations in the concentrations of the three compounds studied were observed, and the results suggest no sorption process, with the compounds being almost entirely biodegraded by the soil sample, or possibly the formation of nonextractable residues could occur.