Halonitromethanes (HNMs) in drinking water are increasingly becoming a public concern due to their high health risks, so development of a sensitive method for their analysis has become a priority. Liquid–liquid extraction (LLE) method is dominantly used in current studies regarding HNMs. However the sensitivity is far from ideal. The present study aims to investigate the factors that may influence the extraction efficiency during HNM analysis by LLE method, and as a result develop a more sensitive extraction method for HNM determination. Results showed that the dose of sodium sulfate exerted the most significant influence, followed by copper sulfate, while the pH and manual shaking times have little effect. Under the suitable conditions (for extracting HNMs in 45 mL water: pH = 3.5–5, CuSO4 = 1.0 g, Na2SO4 = 6 g, shaking times = 120–180), the correlation coefficients (r) of the calibration curves for nine HNMs were all more than 0.9925. The method detection limit (MDL) ranged from 0.017 to 0.217 μg L−1 with an average of 0.076 μg L−1, which was dominantly lower than the method reported. The recovery (spiked blank samples: 98–108%; spiked tap water: 81–120%) and precision (relative standard deviation: 0.46–6.72) also showed good reliability and reproducibility of the method. Finally, the developed method was applied to the determination of HNMs in real water samples.

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