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Trends in Chromatography   Volumes    Volume 8 
Abstract
Experiments for miniaturization and modification of the multi-pesticide residue method EN 12393
Philipp Steinbach, Wolfgang Schwack
Pages: 113 - 129
Number of pages: 17
Trends in Chromatography
Volume 8 

Copyright © 2013 Research Trends. All rights reserved

ABSTRACT
 
With the objective to miniaturize and accelerate EN 12393 sample preparation, extraction, partitioning as well as cleanup by gel permeation chromatography (GPC) were reinvestigated. Different combinations of extraction and partitioning alternatives were tested by joining two extraction and three partitioning techniques to three combinations (dispersing/dispersing; shaking/shaking; sonication/shaking). They were evaluated in terms of applicability to routine analysis and recoveries for spiked and incurred pesticide residues. Compared to EN 12393, the combination shaking/shaking and dispersing/dispersing gave comparable results, while the combination sonication/shaking provided slightly lower recoveries, especially for incurred residues. As shaking/shaking is more convenient for routine analysis, it was selected as the preferred combination for a miniaturized method. Four high resolution GPC columns were compared with regard to separation of sunflower oil from selected pesticides with the aim to reduce the runtime of the GPC cleanup. The PSS GRAM 30 Å column provided the best performance. Methanol was used as solvent modifier to improve the elution behaviour of polar pesticides, resulting in a runtime of 25 min, which allowed a high sample throughput per column. Together with the miniaturized extraction and partitioning steps, analysis time per sample was reduced by about 30%, while hands-on time was about half as compared to EN 12393.
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