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

In this work, an in situ acylation combined with solid‐phase microextraction coupled to gas chromatography and mass spectrometry method has been developed for simultaneously determining haloanisoles (2,4,6‐trichloranisole, 2,4,6‐tribromoanisole), and their direct precursors (2,4,6‐trichlorophenol, 2,4,6‐tribromophenol) and indirect precursors (2‐chloropenol, 2,4‐dichlorophenol, 2‐bromophenol, 2,4‐dibromophenol) in water. The key parameters for the solid‐phase microextraction were determined by using Plackett–Burman screening and optimized by central composite optimization. Under optimal conditions, the eight compounds can be analyzed in a short time (33 min) with a strong linearity ranging from 2 to 200 ng/L (correlation coefficient greater than 0.996), showing good sensitivities with the limit of detection in a range of 0.23–0.91 ng/L and a limit of quantification of 0.77–3.03 ng/L, good repeatability (2.00–9.10%) and interday precision (1.67–11.3%). When environmental water samples were treated, the recoveries of target compounds were 75.5–127.3%, suggesting that the developed method could be applied in probing the origin of haloanisoles and monitoring halophenols and haloanisoles in natural waters at concentration levels of ng/L.