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Open AccessFeature PaperArticle

New Method for Simultaneous Determination of Microcystins and Cylindrospermopsin in Vegetable Matrices by SPE-UPLC-MS/MS

Area of Toxicology, Faculty of Pharmacy, University of Sevilla, C/Profesor García González 2, 41012 Sevilla, Spain
CIIMAR/CIMAR—Interdisciplinary Centre of Marine and Environmental Research, University of Porto, Terminal de Cruzeiros do Porto de leixões, Av General Norton de Matos, 4450-208 Matosinhos, Portugal
Faculty of Sciences, University of Porto, Rua do Campo Alegre, 4169-007 Porto, Portugal
Author to whom correspondence should be addressed.
Toxins 2018, 10(10), 406;
Received: 7 September 2018 / Revised: 3 October 2018 / Accepted: 6 October 2018 / Published: 8 October 2018
(This article belongs to the Special Issue Cyanobacteria and Cyanotoxins: New Advances and Future Challenges)
Cyanotoxins are a large group of noxious metabolites with different chemical structure and mechanisms of action, with a worldwide distribution, producing effects in animals, humans, and crop plants. When cyanotoxin-contaminated waters are used for the irrigation of edible vegetables, humans can be in contact with these toxins through the food chain. In this work, a method for the simultaneous detection of Microcystin-LR (MC-LR), Microcystin-RR (MC-RR), Microcystin-YR (MC-YR), and Cylindrospermopsin (CYN) in lettuce has been optimized and validated, using a dual solid phase extraction (SPE) system for toxin extraction and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for analysis. Results showed linear ranges (5–50 ng g−1 f.w.), low values for limit of detection (LOD) (0.06–0.42 ng g−1 f.w.), and limit of quantification (LOQ) (0.16–0.91 ng g−1 f.w.), acceptable recoveries (41–93%), and %RSDIP values for the four toxins. The method proved to be robust for the three variables tested. Finally, it was successfully applied to detect these cyanotoxins in edible vegetables exposed to cyanobacterial extracts under laboratory conditions, and it could be useful for monitoring these toxins in edible vegetables for better exposure estimation in terms of risk assessment. View Full-Text
Keywords: microcystins; cylindrospermopsin; method validation; UPLC-MS/MS; lettuce microcystins; cylindrospermopsin; method validation; UPLC-MS/MS; lettuce
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Díez-Quijada, L.; Guzmán-Guillén, R.; Prieto Ortega, A.I.; Llana-Ruíz-Cabello, M.; Campos, A.; Vasconcelos, V.; Jos, Á.; Cameán, A.M. New Method for Simultaneous Determination of Microcystins and Cylindrospermopsin in Vegetable Matrices by SPE-UPLC-MS/MS. Toxins 2018, 10, 406.

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