Journal
ENVIRONMENTAL RESEARCH
Volume 185, Issue -, Pages -Publisher
ACADEMIC PRESS INC ELSEVIER SCIENCE
DOI: 10.1016/j.envres.2020.109284
Keywords
Cyanotoxins; Response surface methodology; Box-Behnken design; Method validation; Solid phase extraction; Mussels
Funding
- Spanish Ministry of Economy and Competitiveness [AGL 201564558-R]
- FPI [BES-2016078,773]
- EFSA funding under the EU-FORA Programme
- NORTE 2020 through the ERDF [PTDC/ASP-PES/31762/2017, UID/Multi/04423/2013]
- Portugal 2020 through the ERDF [PTDC/ASP-PES/31762/2017, UID/Multi/04423/2013]
- European Union through the ERDF [PTDC/ASP-PES/31762/2017, UID/Multi/04423/2013]
- Portuguese Science Foundation (Fundacao para a Ciencia e a Tecnologia, FCT)
- Fundação para a Ciência e a Tecnologia [PTDC/ASP-PES/31762/2017] Funding Source: FCT
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The aim of this study was to optimize the extraction conditions of Microcystin-LR (MC-LR), Microcystin-RR (MC-RR), Microcystin-YR (MC-YR) and Cylindrospermopsin (CYN) simultaneously from mussels by using response surface methodology (RSM) and to validate the method by a dual solid phase extraction (SPE) system combined with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The optimal parameters were: 90% MeOH (% v/v) for the extraction, a solvent/sample ratio of 75 and 15% MeOH in the extract before loading onto SPE. Mussels were spiked at 10; 37.5 and 75 ng g(-1) fresh weight (f.w) of the 4 toxins, showing linear ranges of 0.5-75 ng g(-1) f.w; low values for the limits of detection (0.01-0.39 ng g(-1) f.w.) and quantification (0.23-0.40 ng g(-1) f.w.); acceptable recoveries (70.37-114.03%) and relative standard deviation (%RSDIP) values (2.61-13.73%). The method was successfully applied to edible mussels exposed to cyanobacterial extracts under laboratory conditions, and it could allow the monitoring of these cyanotoxins in environmental mussel samples.
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