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Full automatic determination of chlorophenols in water using solid‐phase microextraction/on‐fiber derivatization and gas chromatography‐mass spectrometry
Author(s) -
Wang Xiaowei,
Chen Ruohong,
Luan Tiangang,
Lin Li,
Zou Shichun,
Yang Qingshu
Publication year - 2012
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201100979
Subject(s) - derivatization , solid phase microextraction , chromatography , silylation , chemistry , extraction (chemistry) , mass spectrometry , gas chromatography–mass spectrometry , reagent , sample preparation , fiber , detection limit , gas chromatography , desorption , solid phase extraction , bstfa , adsorption , organic chemistry , catalysis
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.