Application of comprehensive two-dimensional gas chromatography with nitrogen-selective detection for the analysis of fungicide residues in vegetable samples

Khummueng, W, Trenerry, V, Rose, G and Marriott, P 2006, 'Application of comprehensive two-dimensional gas chromatography with nitrogen-selective detection for the analysis of fungicide residues in vegetable samples', Journal Of Chromatography A, vol. 1131, pp. 203-214.


Document type: Journal Article
Collection: Journal Articles

Title Application of comprehensive two-dimensional gas chromatography with nitrogen-selective detection for the analysis of fungicide residues in vegetable samples
Author(s) Khummueng, W
Trenerry, V
Rose, G
Marriott, P
Year 2006
Journal name Journal Of Chromatography A
Volume number 1131
Start page 203
End page 214
Total pages 11
Publisher Elsevier Science
Abstract Comprehensive two-dimensional gas chromatography (GCxGC) with nitrogen-phosphorus detection (NPD) has been investigated for the separation and quantitation of fungicides in vegetable samples. The detector gas flows (H-2, N-2 and air) were adjusted to achieve maximum response of signal whilst minimizing peak width. The comparison of different column sets and selection of the temperature program were carried out with a mixture of nine N-containing standard fungicides, eight of which were chlorinated. The results from GCxGC-NPD and GCxGC with micro electron-capture detection (mu ECD) were compared. External calibrations of fungicides were performed over a concentration range from I to 1000 mu g L-1. The peak area calibration curves generally had regression coefficients of R-2 > 0.9980, however for iprodione which was observed to undergo on-column degradation, an R-2 of 0.990 was found. The limit of detection (LOD) and limit of quantitation (LOQ) were less than about 74 and 246 ng L-1, respectively. The intra-day and inter-day RSD values were measured for solutions of concentration 0.100, 0.500 and 1.50 mg L-1. For the 0.500 mg L-1 solution, intra- and inter-day precision of peak area and peak height for most of the pesticides were about 2% and 8%, respectively. Excellent linearity was observed for these standards, from 0.001 to 25.00 mg L-1. The standard mixture peak positions were identified by using GCxGC with quadrupole mass spectrometry (qMS). To illustrate the potential and the versatility of both GCxGC-NPD and GCxGC-mu ECD, the method was applied to determination of fungicides in a vegetable extract. Decomposition of one fungicide standard (iprodione) during chromatography elation was readily observed in the two-dimensional (2D) GCxGC plot as a diagonal ridge response in the 2D chromatogram between the degrading compound and the decomposition product.
Subject Separation Science
DOI - identifier 10.1016/j.chroma.2006.07.035
Copyright notice Copyright © 2006 Elsevier B.V. All rights reserved.
ISSN 0021-9673
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