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Environmental problems - Chemical approaches
RESEARCH ARTICLE (Open Access)

Determination of inorganic As, DMA and MMA in marine and terrestrial tissue samples: a consensus extraction approach

Zuzana Gajdosechova https://orcid.org/0000-0002-6174-181X A * , Patricia Grinberg https://orcid.org/0000-0002-1167-6474 A , Kevin Kubachka B , Mesay Wolle https://orcid.org/0000-0001-5586-6643 C , Andrea Raab https://orcid.org/0000-0003-2058-0105 D , Joerg Feldmann https://orcid.org/0000-0002-0524-8254 D , Rebecca Sim https://orcid.org/0000-0001-7398-8062 E F , Ásta H. Pétursdóttir https://orcid.org/0000-0002-6739-0598 E , Tomáš Matoušek https://orcid.org/0000-0002-7603-1773 G , Stanislav Musil https://orcid.org/0000-0001-8003-0370 G , Ben Wozniak H , Stephen Springer H , Nausheen W. Sadiq H , Hakan Gurleyuk H , Calvin H. Palmer A , Indumathi Pihillagawa Gedara A and Zoltan Mester https://orcid.org/0000-0002-2377-2615 A
+ Author Affiliations
- Author Affiliations

A National Research Council Canada, Metrology, 1200 Montreal Road, Ottawa, ON K1A 0R6, Canada.

B Forensic Chemistry Center, Office of Regulatory Science, Office of Regulatory Affairs, U.S. Food and Drug Administration, Cincinnati, OH 45237, USA.

C Division of Bioanalytical Chemistry, Office of Regulatory Science, Center for Food Safety and Applied Nutrition, US Food and Drug Administration, 5001, Campus Drive, College Park, MD 20740, USA.

D Institute for Chemistry, TESLA - Analytical Chemistry, University of Graz, Universitätsplatz 1/I, 8010, Graz, Austria.

E Matís, Research and Innovation, Vinlandsleid 12, 113, Reykjavik, Iceland.

F University of Iceland, School of Engineering and Natural Sciences, Dunhagi 3, 107 Reykjavik, Iceland.

G Institute of Analytical Chemistry of the Czech Academy of Sciences, Veveří 97, 602 00, Brno, Czech Republic.

H Brooks Applied Labs, 18804 North Creek Parkway, Suite 100, Bothell, WA 98011, USA.


Handling Editor: Kevin Wilkinson

Environmental Chemistry 20(2) 5-17 https://doi.org/10.1071/EN23006
Submitted: 13 January 2023  Accepted: 3 April 2023   Published: 4 May 2023

© 2023 The Author(s) (or their employer(s)). Published by CSIRO Publishing. This is an open access article distributed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International License (CC BY-NC-ND)

Environmental context. Arsenic can be found in all environmental compartments in a large number of chemical forms of varying toxicity. We performed an inter-laboratory comparison study focusing on quantitation of some of the most toxic arsenic forms in seven different biological materials and found very good agreement among the submitted results. Certification of the studied materials will provide suitable quality control samples for environmentally relevant concentrations of arsenic in food products and biota.

Rationale. Arsenic (As) speciation analysis in biological matrices has been performed for several decades; however, there are very few matrix certified reference materials available for the validation of analytical methods. The literature data on the mass fractions of As species in the existing certified reference materials are inconsistent and suggest method extraction dependency.

Methodology. In the present study, an international round-robin study was organised to identify the possible sources of discrepancies in quantitation of several As species in different matrices of biological reference materials: one plant tissue, three marine and three terrestrial biological tissues. Each participating laboratory was provided with a set of identical calibration standard solutions, and analysed the samples by following a common group extraction method as well as using an in-house protocol.

Results. The results showed that significant biases can be introduced by insufficient verification of the analyte’s mass fractions in the calibration standard solutions. The choice of extraction method seems to have very little impact on the quantitation of As species in the studied plant and terrestrial biological tissues. However, following a prescribed extraction method led to significant reduction of uncertainties in more complex samples such as marine animal tissues.

Discussion. Some differences in the mass fractions of As species extracted from marine animal tissues in water (with and without H2O2) were observed and should be further investigated. Despite the variety of extraction methods used, very good agreement between reported mass fractions was achieved and the combined consensus values will be published as certified reference values of As species in the studied materials.

Keywords: Arsenic speciation, certified reference material, extraction method, high performance liquid chromatography, hydride generation, inorganic arsenic, marine tissue, mass spectrometry.


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