Abstract

An analytical liquid-liquid extraction-gas chromatography–mass spectrometry (LLE-GC-MS) method was developed for the determination of nine haloacetic acids (HAAs) in water. Under the optimized conditions, the matrix-matched calibration curves of all analytes presented correlation coefficients higher than 0.99 (range level of 2–1000 μg L−1). The LODs and LOQs were <2.6 μg L−1 and <3.9 μgL−1, respectively. The relative standard deviations (RSDs) of the intra and inter-day precisions varied in the ranges of 0.01–7.31% and 1.68–19.07%, respectively. RSDs of the accuracy were 0.02–7.31%, and the recoveries were 79.71–113.22%. The validated method had a comparable LODs to similar previously reported techniques in addition to an enhanced LOQs, precision, accuracy, and recovery. Compared with reported LLE-GC-MS methods, the use of distilled H2SO4 in the methylation reaction using acidic methanol favored the process. The GC run time for HAA analysis was 25.5 min. Finally, the proposed procedure was successfully applied to the determination of low concentrations of dichloroacetic acid and trichloroacetic acid, formed during the chlorination of water in the presence of the cyanobacteria Microcystis aeruginosa.

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