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Methylmercury determination in freshwater biota and sediments: Static headspace GC-MS compared to direct mercury analyzer
We developed and compared two analytical methods for determination of MeHg in freshwater biota and sediments, by: I) simplified static headspace GC-MS using internal standard (IS) isotope dilution quantification, after microwave acid digestion and aqueous phase NaBEt(4) ethylation; II) Automated Mer...
Autores principales: | , , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
Elsevier
2021
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8720905/ https://www.ncbi.nlm.nih.gov/pubmed/35004215 http://dx.doi.org/10.1016/j.mex.2021.101581 |
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author | Valsecchi, Lucia Roscioli, Claudio Schiavon, Alfredo Marziali, Laura |
author_facet | Valsecchi, Lucia Roscioli, Claudio Schiavon, Alfredo Marziali, Laura |
author_sort | Valsecchi, Lucia |
collection | PubMed |
description | We developed and compared two analytical methods for determination of MeHg in freshwater biota and sediments, by: I) simplified static headspace GC-MS using internal standard (IS) isotope dilution quantification, after microwave acid digestion and aqueous phase NaBEt(4) ethylation; II) Automated Mercury Analyzer, after double toluene extraction followed by back-extraction with L-cystein. The performance was evaluated by analysis of certified reference materials. For biota, mean recovery was 100 ± 2% and relative standard deviation (RSD) ≤ 6.8% for method I, and mean recovery was 98 ± 7% and RSD ≤13% for method II. For sediments, recovery of 94.5% and RSD of 8.8% were obtained with method I, and recovery of 90.3% and RSD of 9.4% with method II. Limits of detection (LOD) were 0.7 µg kg(−1) and 6 µg kg(−1), respectively. Both techniques were tested for MeHg analysis in freshwater invertebrates, fish and sediments, covering a large range of MeHg values (1.9–670 µg kg(−1) d.w.). • Both protocols proved to be suitable for MeHg analysis in complex environmental matrices, even if, for method II, interferences in the extraction phase and limited sensitivity may hinder sediment analysis. • Passing-Bablock regression revealed a slight disproportion between methods, with line slope = 1.058 (95% CI ranging from 1.001 to 1.090). |
format | Online Article Text |
id | pubmed-8720905 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2021 |
publisher | Elsevier |
record_format | MEDLINE/PubMed |
spelling | pubmed-87209052022-01-07 Methylmercury determination in freshwater biota and sediments: Static headspace GC-MS compared to direct mercury analyzer Valsecchi, Lucia Roscioli, Claudio Schiavon, Alfredo Marziali, Laura MethodsX Method Article We developed and compared two analytical methods for determination of MeHg in freshwater biota and sediments, by: I) simplified static headspace GC-MS using internal standard (IS) isotope dilution quantification, after microwave acid digestion and aqueous phase NaBEt(4) ethylation; II) Automated Mercury Analyzer, after double toluene extraction followed by back-extraction with L-cystein. The performance was evaluated by analysis of certified reference materials. For biota, mean recovery was 100 ± 2% and relative standard deviation (RSD) ≤ 6.8% for method I, and mean recovery was 98 ± 7% and RSD ≤13% for method II. For sediments, recovery of 94.5% and RSD of 8.8% were obtained with method I, and recovery of 90.3% and RSD of 9.4% with method II. Limits of detection (LOD) were 0.7 µg kg(−1) and 6 µg kg(−1), respectively. Both techniques were tested for MeHg analysis in freshwater invertebrates, fish and sediments, covering a large range of MeHg values (1.9–670 µg kg(−1) d.w.). • Both protocols proved to be suitable for MeHg analysis in complex environmental matrices, even if, for method II, interferences in the extraction phase and limited sensitivity may hinder sediment analysis. • Passing-Bablock regression revealed a slight disproportion between methods, with line slope = 1.058 (95% CI ranging from 1.001 to 1.090). Elsevier 2021-11-18 /pmc/articles/PMC8720905/ /pubmed/35004215 http://dx.doi.org/10.1016/j.mex.2021.101581 Text en © 2021 The Authors. Published by Elsevier B.V. https://creativecommons.org/licenses/by-nc-nd/4.0/This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/). |
spellingShingle | Method Article Valsecchi, Lucia Roscioli, Claudio Schiavon, Alfredo Marziali, Laura Methylmercury determination in freshwater biota and sediments: Static headspace GC-MS compared to direct mercury analyzer |
title | Methylmercury determination in freshwater biota and sediments: Static headspace GC-MS compared to direct mercury analyzer |
title_full | Methylmercury determination in freshwater biota and sediments: Static headspace GC-MS compared to direct mercury analyzer |
title_fullStr | Methylmercury determination in freshwater biota and sediments: Static headspace GC-MS compared to direct mercury analyzer |
title_full_unstemmed | Methylmercury determination in freshwater biota and sediments: Static headspace GC-MS compared to direct mercury analyzer |
title_short | Methylmercury determination in freshwater biota and sediments: Static headspace GC-MS compared to direct mercury analyzer |
title_sort | methylmercury determination in freshwater biota and sediments: static headspace gc-ms compared to direct mercury analyzer |
topic | Method Article |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8720905/ https://www.ncbi.nlm.nih.gov/pubmed/35004215 http://dx.doi.org/10.1016/j.mex.2021.101581 |
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