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 NaBEt4 ethylation; II) Automated Mercu...

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Autores principales:	Lucia Valsecchi, Claudio Roscioli, Alfredo Schiavon, Laura Marziali
Formato:	article
Lenguaje:	EN
Publicado:	Elsevier 2021
Materias:	Organometallic compounds Methylmercury determination Benthic invertebrates Sediments Science Q
Acceso en línea:	https://doaj.org/article/183b715568ca455b817bf9f136cb8922
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spelling	oai:doaj.org-article:183b715568ca455b817bf9f136cb89222021-11-22T04:26:03ZMethylmercury determination in freshwater biota and sediments: Static headspace GC-MS compared to direct mercury analyzer2215-016110.1016/j.mex.2021.101581https://doaj.org/article/183b715568ca455b817bf9f136cb89222021-01-01T00:00:00Zhttp://www.sciencedirect.com/science/article/pii/S221501612100371Xhttps://doaj.org/toc/2215-0161We 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 NaBEt4 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).Lucia ValsecchiClaudio RoscioliAlfredo SchiavonLaura MarzialiElsevierarticleOrganometallic compoundsMethylmercury determinationBenthic invertebratesSedimentsScienceQENMethodsX, Vol 8, Iss , Pp 101581- (2021)
institution	DOAJ
collection	DOAJ
language	EN
topic	Organometallic compounds Methylmercury determination Benthic invertebrates Sediments Science Q
spellingShingle	Organometallic compounds Methylmercury determination Benthic invertebrates Sediments Science Q Lucia Valsecchi Claudio Roscioli Alfredo Schiavon Laura Marziali Methylmercury determination in freshwater biota and sediments: Static headspace GC-MS compared to direct mercury analyzer
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 NaBEt4 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	article
author	Lucia Valsecchi Claudio Roscioli Alfredo Schiavon Laura Marziali
author_facet	Lucia Valsecchi Claudio Roscioli Alfredo Schiavon Laura Marziali
author_sort	Lucia Valsecchi
title	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_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_sort	methylmercury determination in freshwater biota and sediments: static headspace gc-ms compared to direct mercury analyzer
publisher	Elsevier
publishDate	2021
url	https://doaj.org/article/183b715568ca455b817bf9f136cb8922
work_keys_str_mv	AT luciavalsecchi methylmercurydeterminationinfreshwaterbiotaandsedimentsstaticheadspacegcmscomparedtodirectmercuryanalyzer AT claudioroscioli methylmercurydeterminationinfreshwaterbiotaandsedimentsstaticheadspacegcmscomparedtodirectmercuryanalyzer AT alfredoschiavon methylmercurydeterminationinfreshwaterbiotaandsedimentsstaticheadspacegcmscomparedtodirectmercuryanalyzer AT lauramarziali methylmercurydeterminationinfreshwaterbiotaandsedimentsstaticheadspacegcmscomparedtodirectmercuryanalyzer
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Methylmercury determination in freshwater biota and sediments: Static headspace GC-MS compared to direct mercury analyzer

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