Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1218, Issue 2, Pages 303-315Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2010.11.010
Keywords
Screening; Water samples; Gas chromatography; Time-of-flight mass spectrometry; Qualitative validation; Organic pollutants
Funding
- Spanish Ministry of Science and Education [CTQ2009-12347]
- Generalitat Valenciana [PROMETEO/2009/054]
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In this work, a multiclass screening method for organic contaminants in natural and wastewater has been developed and validated for qualitative purposes, i.e. to ensure the reliable and sensitive identification of compounds detected in samples at a certain level of concentration. The screening is based on the use of GC-TOFMS, and the sample procedure involves solid phase extraction with C-18 cartridges. Around 150 organic contaminants from different chemical families were investigated, including PAHs, octyl/nonyl phenols, PCBs, PBDEs and a notable number of pesticides, such as insecticides (organochlorines, organophosphorus, carbamates and pyrethroids), herbicides (triazines and chloroacetanilides), fungicides and several relevant metabolites. Surface water, ground water and effluent wastewater were spiked with all target analytes at three concentration levels (0.02, 0.1 and 1 mu g/L). Influent wastewater and raw leachate from a municipal solid waste treatment plant were spiked at two levels (0.1 and 1 mu g/L). Up to five m/z ions were evaluated for every compound. The identification criterion was the presence of, at least, two m/z ions at the expected retention time, measured at their accurate mass, and the accomplishment of the Q/qi intensity ratio within specified tolerances. The vast majority of compounds investigated were correctly identified in the samples spiked at 1 mu g/L.. When analyte concentration was lowered down to 0.1 mu g/L the identification was more problematic, especially in complex-matrix samples like influent wastewater. On the contrary, many contaminants could be properly identified at the lowest level 0.02 mu g/L in cleaner matrices. The procedure was applied to the screening of water samples of different origin and matrix composition and allowed the detection of several target contaminants. A highly reliable identification could be carried out thanks to the sensitive full-spectrum acquisition at accurate mass, the high selectivity reached with the use of narrow-mass window extracted ion chromatograms, the low mass errors observed in the positive detections and the Q/q ratio accomplishment. (C) 2010 Elsevier B.V. All rights reserved.
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