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

Abstract

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 Na2 CO3 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 (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.

A Review on Extraction Solvents in the Dispersive Liquid-Liquid Microextraction

“…In addition, higher recovery efficiency with lower relative standard deviation can also be achieved by means of using only 1methyl-3-bromobutane as extraction solvent without having to rely on dispersive solvent, which is capable of reducing the use of organic solvent [28]. [35], isooctane [36], and 1-dodecanol [37] and 1-undecanol [38] have been used as extraction solvents in low-density solvents (LDS) DLLME. In addition, they have been proven to possess low LOD and LOQ, high recovery and higher linearity.…”

Simultaneous determination of haloanisoles and halophenols in water using in situ acylation combined with solid‐phase microextraction with gas chromatography and mass spectrometry

“…As for the extraction step, several approaches to the quantitative determination of haloanisoles and halophenols have been reported, such as LLE [22,23], SFE [24], SPE [8], SPME [25][26][27][28], stir bar sorptive extraction (SBSE) [14,29], dispersive liquid-liquid microextraction (DLLME) [17,30,31], ultrasound-assisted emulsification microextraction (USAEME) [16], and vortex-assisted liquid-liquid microextraction (VALLME) [4]. These methods also played important roles in shortening the operational time (DLLME, USAEME, and, VALLME) or reducing manual operation (SPE, SPME, and SBSE).…”

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“…The choice of lower-density organic solvent is more popular than high-density solvents [31]. The low-density solvents such as n-hexane [30], toluene [32], 2-ethyl-1-hexanol [31], 1-heptanol [34], 1-octanol [35], isooctane [36], and 1-dodecanol [37] and 1-undecanol [38] have been used as extraction solvents in low-density solvents (LDS) DLLME. In addition, they have been proven to possess low LOD and LOQ, high recovery and higher linearity.…”