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

Abstract

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.

Dispersive liquid‐liquid microextraction coupled with pressure‐assisted electrokinetic injection for simultaneous enrichment of seven phenolic compounds in water samples followed by determination using capillary electrophoresis

“…Considering their low concentration presented in complicated matrices, a number of pretreatment approaches have been developed to concentrate phenolic compounds, such as hollow fiber supported liquid‐liquid liquid membrane microextraction , SPE , dispersive solid phase extraction , SPME , dispersive liquid‐liquid microextraction (DLLME) and cloud point extraction . Moreover, various detection technologies have been applied for analysis of phenolic compounds including HPLC , CE , and GC coupled with UV, fluorescence, and MS detectors.…”

Dispersive liquid–liquid microextraction as a novel enrichment approach for compound-specific carbon isotope analysis of chlorinated phenols

“…It should be noted at this point that we partially observed higher RSD for the measured peak areas compared to studies on the quantification of (chlorinated) phenols by DLLME 33 and other microextraction techniques, such as SPME. 56 However, in contrast to these studies we were primarily interested in the determination of reproducible δ 13 C values. Consequently, a slightly lower reproducibility of peak areas is not problematic as long as the analyzed samples are within the linear range of the IRMS, which is characterized by the independence of the measured δ 13 C value from the injected analyte mass/the peak area.…”

Rapid determination of 14 odorous compounds in drinking water using gas chromatography-mass spectrometry coupled with headspace solid-phase microextraction pretreatment

“…These values were superior to them obtained by previous reports with GC-MS methods, 22,23 and even could be comparable to the LOD values using GC-MS coupling with the procedure of derivatization. 24 The LODs were below their odor thresholds, which were satised with the need for odor monitoring and identication in water.…”