期刊
JOURNAL OF SEPARATION SCIENCE
卷 28, 期 17, 页码 2301-2305出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.200500085
关键词
aldehydes; derivatization; gas chromatography-mass spectrometry; headspace single-drop microextraction with in-drop derivatization; solvent microextraction
A new technique, headspace single-drop microextraction (HS-SDME) with in-drop derivatization, was developed. Its feasibility was demonstrated by analysis of the model compounds, aldehydes in water. A hanging microliter drop of solvent containing the derivatization agent of O-2,3,4,5,6-(pentaflurobenzyl) hydroxylamine hydrochloride (PFBHA) was shown to be an excellent extraction, concentration, and derivatization medium for headspace analysis of aldehydes by GC-MS. Using the microdrop solvent with PFBHA, acetaldehyde, propanal, butanal, hexanal, and heptanal in water were headspace extracted and simultaneously derivatized. The formed oximes in the microdrop were analyzed by GC-MS. HS-SIDME and in-drop derivatization parameters (extraction solvent, extraction temperature, extraction time, stirring rate microdrop volume, and the headspace volume) and the method validations (linearity, precision, detection limit, and recovery) were studied. Compared to liquid-liquid extraction and solid-phase microextraction, HS-SIDME with in-drop derivatization is a simple, rapid, convenient, and inexpensive sample technique.
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