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Analytical methodologies based on LC–MS/MS for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge
In this work, two analytical methodologies based on liquid chromatography coupled to tandem mass spectrometry (LC–MS/MS) were developed for quantification of emerging pollutants identified in sewage sludge after a previous wide-scope screening. The target list included 13 emerging contaminants (EC):...
Autores principales: | , , , , , , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
Elsevier
2016
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4865632/ https://www.ncbi.nlm.nih.gov/pubmed/27222823 http://dx.doi.org/10.1016/j.mex.2016.04.010 |
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author | Boix, C. Ibáñez, M. Fabregat-Safont, D. Morales, E. Pastor, L. Sancho, J.V. Sánchez-Ramírez, J.E. Hernández, F. |
author_facet | Boix, C. Ibáñez, M. Fabregat-Safont, D. Morales, E. Pastor, L. Sancho, J.V. Sánchez-Ramírez, J.E. Hernández, F. |
author_sort | Boix, C. |
collection | PubMed |
description | In this work, two analytical methodologies based on liquid chromatography coupled to tandem mass spectrometry (LC–MS/MS) were developed for quantification of emerging pollutants identified in sewage sludge after a previous wide-scope screening. The target list included 13 emerging contaminants (EC): thiabendazole, acesulfame, fenofibric acid, valsartan, irbesartan, salicylic acid, diclofenac, carbamazepine, 4-aminoantipyrine (4-AA), 4-acetyl aminoantipyrine (4-AAA), 4-formyl aminoantipyrine (4-FAA), venlafaxine and benzoylecgonine. The aqueous and solid phases of the sewage sludge were analyzed making use of Solid-Phase Extraction (SPE) and UltraSonic Extraction (USE) for sample treatment, respectively. The methods were validated at three concentration levels: 0.2, 2 and 20 μg L(−1) for the aqueous phase, and 50, 500 and 2000 μg kg(−1) for the solid phase of the sludge. In general, the method was satisfactorily validated, showing good recoveries (70–120%) and precision (RSD < 20%). Regarding the limit of quantification (LOQ), it was below 0.1 μg L(−1) in the aqueous phase and below 50 μg kg(−1) in the solid phase for the majority of the analytes. The method applicability was tested by analysis of samples from a wider study on degradation of emerging pollutants in sewage sludge under anaerobic digestion. The key benefits of these methodologies are: • SPE and USE are appropriate sample procedures to extract selected emerging contaminants from the aqueous phase of the sewage sludge and the solid residue. • LC–MS/MS is highly suitable for determining emerging contaminants in both sludge phases. • Up to our knowledge, the main metabolites of dipyrone had not been studied before in sewage sludge. |
format | Online Article Text |
id | pubmed-4865632 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2016 |
publisher | Elsevier |
record_format | MEDLINE/PubMed |
spelling | pubmed-48656322016-05-24 Analytical methodologies based on LC–MS/MS for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge Boix, C. Ibáñez, M. Fabregat-Safont, D. Morales, E. Pastor, L. Sancho, J.V. Sánchez-Ramírez, J.E. Hernández, F. MethodsX Environmental Science In this work, two analytical methodologies based on liquid chromatography coupled to tandem mass spectrometry (LC–MS/MS) were developed for quantification of emerging pollutants identified in sewage sludge after a previous wide-scope screening. The target list included 13 emerging contaminants (EC): thiabendazole, acesulfame, fenofibric acid, valsartan, irbesartan, salicylic acid, diclofenac, carbamazepine, 4-aminoantipyrine (4-AA), 4-acetyl aminoantipyrine (4-AAA), 4-formyl aminoantipyrine (4-FAA), venlafaxine and benzoylecgonine. The aqueous and solid phases of the sewage sludge were analyzed making use of Solid-Phase Extraction (SPE) and UltraSonic Extraction (USE) for sample treatment, respectively. The methods were validated at three concentration levels: 0.2, 2 and 20 μg L(−1) for the aqueous phase, and 50, 500 and 2000 μg kg(−1) for the solid phase of the sludge. In general, the method was satisfactorily validated, showing good recoveries (70–120%) and precision (RSD < 20%). Regarding the limit of quantification (LOQ), it was below 0.1 μg L(−1) in the aqueous phase and below 50 μg kg(−1) in the solid phase for the majority of the analytes. The method applicability was tested by analysis of samples from a wider study on degradation of emerging pollutants in sewage sludge under anaerobic digestion. The key benefits of these methodologies are: • SPE and USE are appropriate sample procedures to extract selected emerging contaminants from the aqueous phase of the sewage sludge and the solid residue. • LC–MS/MS is highly suitable for determining emerging contaminants in both sludge phases. • Up to our knowledge, the main metabolites of dipyrone had not been studied before in sewage sludge. Elsevier 2016-04-27 /pmc/articles/PMC4865632/ /pubmed/27222823 http://dx.doi.org/10.1016/j.mex.2016.04.010 Text en © 2016 The Author(s) http://creativecommons.org/licenses/by/4.0/ This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/). |
spellingShingle | Environmental Science Boix, C. Ibáñez, M. Fabregat-Safont, D. Morales, E. Pastor, L. Sancho, J.V. Sánchez-Ramírez, J.E. Hernández, F. Analytical methodologies based on LC–MS/MS for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge |
title | Analytical methodologies based on LC–MS/MS for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge |
title_full | Analytical methodologies based on LC–MS/MS for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge |
title_fullStr | Analytical methodologies based on LC–MS/MS for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge |
title_full_unstemmed | Analytical methodologies based on LC–MS/MS for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge |
title_short | Analytical methodologies based on LC–MS/MS for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge |
title_sort | analytical methodologies based on lc–ms/ms for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge |
topic | Environmental Science |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4865632/ https://www.ncbi.nlm.nih.gov/pubmed/27222823 http://dx.doi.org/10.1016/j.mex.2016.04.010 |
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