title: 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.
authors.affiliation: MOE Key Laboratory of Aquatic Product Safety, School of Life Sciences, Sun Yat-sen University, Guangzhou, P R China.
authors.forename: Xiaowei
authors.initials: X
authors.lastname: Wang
authors.forename: Ruohong
authors.initials: R
authors.lastname: Chen
authors.forename: Tiangang
authors.initials: T
authors.lastname: Luan
authors.forename: Li
authors.initials: L
authors.lastname: Lin
authors.forename: Shichun
authors.initials: S
authors.lastname: Zou
authors.forename: Qingshu
authors.initials: Q
authors.lastname: Yang
mesh_terms: D001331:Automation; D002733:Chlorophenols / Q000032:analysis* / Q000302:isolation & purification*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D045483:Rivers / Q000737:chemistry; D052617:Solid Phase Microextraction / Q000295:instrumentation / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification*
chemical_list: D002733:Chlorophenols; D014874:Water Pollutants, Chemical