期刊
JOURNAL OF CHROMATOGRAPHY A
卷 963, 期 1-2, 页码 137-148出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/S0021-9673(02)00646-5
关键词
factorial design; water analysis; solid-phase microextraction; headspace analysis; phenols; chlorophenols; alkylphenols; cresols
Solid-phase microextraction (SPME) coupled to gas chromatography-mass spectrometry has been applied to the extraction of 30 phenol derivatives from water samples. Analytes were in situ acetylated and headspace solid-phase microextraction was performed. Different parameters affecting extraction efficiency were studied. Optimization of temperature, type of microextraction fiber and volume of sample has been done by means of a mixed-level categorical experimental design, which allows to study main effects and second order interactions. Five different fiber coatings were employed in this study; also, extraction temperature was studied at three levels. Both factors, fiber coating and extraction temperature, were important to achieve high sensitivity. Moreover, these parameters showed a significant interaction, which indicates the different kinetic behavior of the SPME process when different coatings are used. It was found that 75 mum carboxen-polydimethylsiloxane and 100 mum polydimethylsiloxane, yield the highest responses. The first one is specially appropriated for phenol, methylphenols and low chlorinated chlorophenols and the second one for highly chlorinated phenols. The two methods proposed in this study shown good linearity and precision. Practical applicability was demonstrated through the analysis of a real sewage water sample, contaminated with phenols. (C) 2002 Elsevier Science B.V. All rights reserved.
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