Headspace single-drop microextraction with in-drop derivatization for aldehyde analysis

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‐(pentafluroben...

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Bibliographic Details
Published in:Journal of separation science 2005-11, Vol.28 (17), p.2301-2305
Main Authors: Deng, Chunhui, Yao, Ning, Li, Ning, Zhang, Xiangmin
Format: Article
Language:English
Subjects:
Aldehydes
Analytical chemistry
Applied sciences
Chemistry
Chromatographic methods and physical methods associated with chromatography
Derivatization
Exact sciences and technology
Gas chromatographic methods
Gas chromatography-mass spectrometry
Headspace single-drop microextraction with in-drop derivatization
Other wastewaters
Pollution
Solvent microextraction
Wastewaters
Water treatment and pollution
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Summary: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‐SDME 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‐SDME with in‐drop derivatization is a simple, rapid, convenient, and inexpensive sample technique.
ISSN:1615-9306
1615-9314
DOI:10.1002/jssc.200500085