Scheda di dettaglio – i prodotti della ricerca

DatoValore
TitleMethylmercury determination in freshwater biota and sediments: Static headspace GC-MS compared to direct mercury analyzer
AbstractWe 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 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 and 6 µg kg, 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 d.w.). o 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. o Passing-Bablock regression revealed a slight disproportion between methods, with line slope = 1.058 (95% CI ranging from 1.001 to 1.090).
SourceMethodsX 8
KeywordsBenthic invertebratesMethylmercury determinationMethylmercury in freshwater biota and sediments by GC-MS or automatic mercury analyzerOrganometallic compoundsSediments
JournalMethodsX
Editor, ,
Year2021
TypeArticolo in rivista
DOI10.1016/j.mex.2021.101581
AuthorsValsecchi, Lucia; Roscioli, Claudio; Schiavon, Alfredo; Marziali, Laura
Text461565 2021 10.1016/j.mex.2021.101581 Scopus 2 s2.0 85119410333 Benthic invertebrates Methylmercury determination Methylmercury in freshwater biota and sediments by GC MS or automatic mercury analyzer Organometallic compounds Sediments Methylmercury determination in freshwater biota and sediments Static headspace GC MS compared to direct mercury analyzer Valsecchi, Lucia; Roscioli, Claudio; Schiavon, Alfredo; Marziali, Laura Istituto di Ricerca sulle Acque, Italy; Leibniz Institute of Freshwater Ecology and Inland Fisheries 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 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 and 6 µg kg, 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 d.w. . o 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. o Passing Bablock regression revealed a slight disproportion between methods, with line slope = 1.058 95% CI ranging from 1.001 to 1.090 . 8 Published version https //doi.org/10.1016/j.mex.2021.101581 Articolo in rivista 2215 0161 MethodsX MethodsX lucia.valsecchi VALSECCHI LUCIA SCHIAVON ALFREDO claudiogiovanni.roscioli ROSCIOLI CLAUDIO GIOVANNI laura.marziali MARZIALI LAURA DTA.AD002.129.001 LAGO MAGGIORE BRUGHERIO