John Wiley & Sons, Ltd.

Development and validation of an in‐house quantitative analysis method for cylindrospermopsin using HILIC liquid chromatography tandem mass spectrometry: Quantification demonstrated in four aquatic organisms

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The cyanobacterial toxin, cylindrospermopsin (CYN), is of great concern in aquatic environments due to its incidence, multiple toxicity endpoints and therefore the severity of health implications. CYN may bioaccumulate in aquatic food webs resulting in high exposure concentrations to higher‐order trophic levels, particularly humans. Due to accumulation at primary levels resulting from exposure to trace amounts of toxin, a sensitive analytical technique with proven aquatic applications is required. Herewith, a HILIC liquid chromatography tandem mass spectrometry method with a lower limit of detection of 200 fg on column (S/N = 3, n = 9) and lower limit of quantification of 1 pg on column (S/N = 11, n = 9) with demonstrated application in four aquatic organisms is described. The analytical method was optimized and validated with a linear range (r2 = 0.999) from 0.1 to 100 ng mL−1 CYN. Mean recovery of the extraction method was 98 ± 2%. Application of the method was demonstrated by quantifying CYN uptake in Scenedesmus subspicatus (green algae), Egeria densa (Brazilian waterweed), Daphnia magna (water flea), and Lumbriculus variegatus (blackworm) after 24 hours of static exposure to 50 µg L−1 CYN. The uptake ranged from 0.05 to 0.11% of the nominal CYN exposure amount. This constitutes a sensitive and reproducible method for extraction and quantification of unconjugated CYN with demonstrated application in four aquatic organisms, which can be used in further aquatic toxicology investigations. This article is protected by copyright. All rights reserved

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