Effect of background derivatization on the signal enhancement of pesticide residues extracted from edible oils

The effect of background derivatization on the signal enhancement of pesticide residues extracted from edible oil samples was studied by GC with negative chemical ionization MS. The analytes were extracted by a solvent extraction process, and the extract was subjected to rapid low‐temperature fat pr...

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Bibliographic Details
Published in:Journal of separation science 2013-12, Vol.36 (24), p.3926-3933
Main Authors: Deme, Pragney, Azmeera, Tirupathi, Bethala, Prabhavathi Devi L.A., Jonnalagadda, Padmaja R., Rachapudi, Prasad B.N., Upadhyayula, Vijaya Sarathi V.R.
Format: Article
Language:English
Subjects:
Biological and medical sciences
Derivatization
Edible
Edible oils
Fat industries
Food industries
Fundamental and applied biological sciences. Psychology
Gas chromatography
Gas Chromatography-Mass Spectrometry
Mass spectrometry
Negative chemical ionization
Pesticide residues
Pesticide Residues - analysis
Pesticide Residues - chemistry
Pesticide Residues - isolation & purification
Pesticides
Plant Oils - chemistry
Plants, Edible - chemistry
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Summary:The effect of background derivatization on the signal enhancement of pesticide residues extracted from edible oil samples was studied by GC with negative chemical ionization MS. The analytes were extracted by a solvent extraction process, and the extract was subjected to rapid low‐temperature fat precipitation. The residual fatty acids were silylated by derivatization with N,O‐bis(trimethylsilyl)trifluoroacetamide. The chromatograms obtained from the derivatized samples showed higher signal intensity and lower detection levels when compared to the direct analysis without derivatization. The sensitivity levels of the method are either better or comparable to that of previously reported methodologies. The LODs of the analyzed organochlorine, organophosphorus, and synthetic pyrethroid residues in sunflower, rice bran, and ground oil samples were in the range of 0.02–0.5 ng/g, and the LOQs were in the range of 0.1–2 ng/g. The intraday and interday accuracies were in the range of 81–116% with RSDs less than 14%. The recoveries obtained were in the range of 53–89% with the RSD values less than 13% for all the studied pesticide residues.
ISSN:1615-9306
1615-9314
DOI:10.1002/jssc.201300454