Citation: CHEN Lihui, JIA Yuzhu, ZHANG Bin, PAN Qiuren, CHEN Qinqin, CAI Weipeng. Determination of cylindrospermopsin, nodularin and microcystins in freshwater fish by dispersive solid phase extraction-liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2019, 37(7): 723-728. doi: 10.3724/SP.J.1123.2019.01022 shu

Determination of cylindrospermopsin, nodularin and microcystins in freshwater fish by dispersive solid phase extraction-liquid chromatography-tandem mass spectrometry

Xiamen Municipal Center for Disease Control and Prevention, Xiamen 361021, China

Received Date: 15 January 2019

Fund Project: Natural Science Foundation Youth Innovation Project in Fujian Province (No. 2016D022).

A method was developed for the determination of cylindrospermopsin (CYN), nodularin (NOD), microcystin-RR (MC-RR), microcystin-YR (MC-YR) and microcystin-LR (MC-LR) in freshwater fish by dispersive solid phase extraction-liquid chromatography-tandem mass spectrometry (DSPE-LC-MS/MS). The analytes were extracted from fish tissues with acetonitrile-water-formic acid (89:10:1, v/v/v), and purified by DSPE using C₁₈ as the adsorbent. The separation of analytes was performed on an Agilent ZORBAX Eclipse XDB C₁₈ column with the gradient elution of acetonitrile and water as mobile phases. Qualitative analysis was performed using the multiple reaction monitoring (MRM) mode. The analytes were quantified by matrix-matched external standard curves. The chromatographic and MS parameters were optimized. Major factors affecting the extraction and cleanup efficiencies including the type of extraction solvent and cleanup sorbent were investigated. The linear correlation coefficients (R²) of the five target compounds were no less than 0.9954. The limits of detection (LODs, S/N=3) and limits of quantification (LOQs, S/N=10) of the five target compounds were 5-10 μg/kg and 15-40 μg/kg, respectively. The spiked recoveries of the five target compounds ranged from 62.3% to 101.2%. The developed method is simple, rapid, accurate, sensitive, and is suitable for the determination of cylindrospermopsin, nodularin and microcystins in freshwater fish.
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