Simultaneous dispersive liquid-liquid microextraction based on a low-density solvent and derivatization followed by gas chromatography for the simultaneous determination of chloroanisoles and the precursor 2,4,6-trichlorophenol in water samples

Chloroanisoles, particularly 2,4,6-trichloroanisole, are commonly identified as major taste and odor compounds in water. In the present study, a simple and efficient method was established for the simultaneous determination of chloroanisoles and the precursor 2,4,6-trichlorophenol in water by using low-density-solvent-based simultaneous dispersive liquid-liquid microextraction and derivatization followed by gas chromatography with electron capture detection. 2,4-Dichloroanisole, 2,6-dichloroanisole, 2,4,6-trichloroanisole, 2,3,4-trichloroanisole, and 2,3,6-trichloroanisole were the chloroanisoles evaluated. Several important parameters of the extraction-derivatization procedures, including the types and volumes of extraction solvent and disperser solvent, concentrations of derivatization agent and base, salt addition, extraction-derivatization time, and temperature were optimized. Under the optimized conditions (80 mu L of isooctane as extraction solvent, 500 mu L of methanol as disperser solvent, 60 mu L of acetic anhydride as derivatization agent, 0.75% of Na2CO3 addition w/v, extraction-derivatization temperature of 25 degrees C, without salt addition), a good linearity of the calibration curve was observed by the square of correlation coefficients (R-2) ranging from 0.9936 to 0.9992. Repeatability and reproducibility of the method were < 4.5% and < 7.3%, respectively. Recovery rates ranged from 85.2 to 101.4%, and limits of detection ranged from 3.0 to 8.7 ng/L. The proposed method was applied successfully for the determination of chloroanisoles and 2,4,6-trichlorophenol in water samples.