Full automatic determination of chlorophenols in water using solid‐phase microextraction/on‐fiber derivatization and gas chromatography‐mass spectrometry

Abstract

A fully automated combination of solid-phase microextraction and on-fiber derivatization coupled with gas chromatography-mass spectrometry was developed to determine 17 chlorophenols in aqueous samples. Optimal parameters for the automated process, such as fiber coating (polyacrylate), derivatization reagent (N,O-bis(trimethylsilyl) trifluoroacetamide), extraction time (60 min), derivatization time (5 min), incubation temperature (35°C), sample pH (3), and ionic strength (300 g L(-1) of NaCl), as well as desorption time (5 min) and desorption temperature (270°C) were established. The whole procedure took only 90 min and was performed automatically. The shortcomings of silylation derivatives, like incompleteness and instability, were overcome by using solid-phase microextraction on-fiber silylation in this study. The results from both pure water and river water samples showed that the method had a good linearity (r(2) = 0.9993-1.0000), ranging from 0.01 to 100 μg L(-1). The related standard deviations were between 3.6 and 10.0%. The limits of detections and qualifications ranged from 0.03 to 3.11 ng L(-1) and 0.09 to 10.4 ng L(-1) for the CPs, respectively. The proposed method is superior to traditional solid phase extraction procedure.

Determination of chlorophenols in water using dispersive liquid–liquid microextraction coupled with water‐in‐oil microemulsion electrokinetic chromatography in normal stacking mode

“…The concentration of chlorophenols in the aquatic environment is low and thus, sample preparation is necessary before instrumental analysis. Various pretreatment techniques including SPE , SPME , LPME have been attempted to extract chlorophenols from water samples. As a mode of LPME, dispersive liquid–liquid microextraction (DLLME) has been widely applied in determining analytes at trace levels in the environmental, food, and biological samples due to its obvious excellence of high enrichment factor, simplicity, rapidness, and low cost .…”

Trace-level screening of dichlorophenols in processed dairy milk by headspace gas chromatography

“…Note the severe tailing of 2,4‐dichlorophenol and the strong adsorption of 2,6‐dichlorophenol by the stationary phase involved. To mitigate this limitation and to improve the chromatographic performance and reliability, it is a common practice for analysts to convert chlorinated phenols to their respective derivatives by derivatization especially for ultra‐trace analysis . However, the incorporation of derivation adds an extra step in sample preparation and often results in another level of complexity to the analytical method.…”

Assessment of anthropogenic pollution by monitoring occurrence and distribution of chemicals in the river Liffey in Dublin

“…6 Levels of aliphatic compounds near the mouth of the river on four sampling days toxicity reported values were 3,198, 5,470 and 3,732 μg L −1 to Chlorella, Daphnia and Tilapia, respectively. On the other hand, this compound has been quantified by other authors (Wang et al 2012) in samples from the Pearl River in China where levels between 0.021 and 0.205 μg L −1 were detected. Alkylphenol compounds, 2,4-dimethylphenol and methyl phenol, were present in the samples (> 70%) at an average concentration of 0.15 and 0.12 μg L −1 , respectively.…”