Development and Validation of a Liquid Chromatography-Tandem Mass Spectrometry Method for the Quantitation of Microcystins in Blue-Green Algal Dietary Supplements

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• 作者：Christine H. Parker ; Whitney L. Stutts ; Stacey L. DeGrasse
• 刊名：Journal of Agricultural and Food Chemistry
• 出版年：2015
• 出版时间：December 2, 2015
• 年：2015
• 卷：63
• 期：47
• 页码：10303-10312
• 全文大小：585K
• ISSN：1520-5118

文摘

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous detection and quantitation of seven microcystin congeners (1鈥?b>7) and nodularin-R (8) in blue-green algal dietary supplements. Single-laboratory method validation data were collected in four supplement matrices (capsule, liquid, powder, and tablet) fortified at toxin concentrations from 0.25鈥?.00 渭g/g (ppm). Average recoveries and relative standard deviations (RSD) using matrix-corrected solvent calibration curves were 101% (6% RSD) for all congeners and supplements investigated. Limits of detection (0.006鈥?.028 渭g/g) and quantitation (0.018鈥?.084 渭g/g) were sufficient to confirm the presence of microcystin contamination at the Oregon-mandated guidance concentration of 1.0 渭g of microcystin-LR_eq/g. Quantitated concentrations of microcystin contamination in market-available Aphanizomenon flos-aquae blue-green algal supplements ranged from 0.18鈥?.87 渭g of microcystin-LR_eq/g for detected congeners microcystin-LR, microcystin-LA, and microcystin-LY (3鈥?b>5). Microcystin-RR, -YR, -LW, and -LF and nodularin-R (1, 2, and 6鈥?) were not detected in the supplements examined.