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

• Published in: Journal of separation science Vol. 39; no. 11; pp. 2146 - 2155
• Main Authors: Bai, Xiuzhi, Zhang, Ting, Li, Haipu, Yang, Zhaoguang
• Format: Journal Article
• Language: English
• Published: Germany Blackwell Publishing Ltd 01.06.2016; Wiley Subscription Services, Inc
• Subjects: 2,4,6‐Trichloroanisole; 2,4,6‐Trichlorophenol; 6-Trichloroanisole; 6-Trichlorophenol; Chromatography; Dispersion; Dispersive liquid-liquid microextraction; Gas chromatography; Gas chromatography with electron capture detection; Liquid-liquid extraction; Methyl alcohol; Precursors; Reagents; Reproducibility; Solvents; Water pollution; 2,4,6-Trichlorophenol; Dispersive liquid-liquid microextraction; 2,4,6-Trichloroanisole; Gas chromatography with electron capture detection
• ISSN: 1615-9306; 1615-9314
• DOI: 10.1002/jssc.201600098

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 μL of isooctane as extraction solvent, 500 μL of methanol as disperser solvent, 60 μL of acetic anhydride as derivatization agent, 0.75% of Na2CO3 addition w/v, extraction‐derivatization temperature of 25°C, without salt addition), a good linearity of the calibration curve was observed by the square of correlation coefficients (R2) 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.