期刊
TALANTA
卷 80, 期 5, 页码 2076-2082出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.talanta.2009.11.008
关键词
Phthalates; Solid-phase microextraction; Gas chromatography ion trap-mass spectrometry; Oil matrices
A solvent-free analytical approach based on headspace solid-phase microextraction (SPME) of oil matrices heated at high temperatures coupled to gas chromatography with mass spectrometry detector (GC-Ion trap) has been developed for the determination of phthalic acid esters (PAEs) in oil matrices without sample manipulation For this study, three fibers. i.e, 85 mu m-polyacrylate (PA), 50/30 mu m-divinylbenzene-carboxen-polydimethylsiloxane (DVB/CAR/PDMS) and 100 mu m-polydimethylsiloxane (PDMS) were tested Variables affecting the SPME headspace composition such as incubation sample temperature, sample incubation time and fiber exposition time were optimized. The optimal values found were 250 degrees C for sample incubation temperature and 30 min for incubation and extraction time. PA fiber was not suitable for the lightest polar phthalates which showed poor extraction and repeatability values. PDMS fiber had very poor response for some of the heavier and non-polar phthalates, whereas DVB/CAR/PDMS fiber showed the best response and repeatability values for the majority of the phthalates studied. The main benefit of the analytical method proposed is the absence of sample manipulation and hence avoidance of possible contamination coming from glassware, environment, solvents and samples. (C) 2009 Elsevier B V. All rights reserved.
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