Journal
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
Volume 57, Issue 16, Pages 7213-7220Publisher
AMER CHEMICAL SOC
DOI: 10.1021/jf901086q
Keywords
Ergot alkaloids; LC-MS; quantitation; vein tissue
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A liquid chromatography-mass spectrometry (LC-MS) method for simultaneous quantitation of seven ergot alkaloids (lysergic acid, ergonovine, ergovaline, ergocornine, ergotamine, ergocryptine, and ergocristine) in vascular tissue was developed and validated. Reverse-phase chromatography, Coupled to an electrospray ionization source, was used to separate and ionize alkaloids. Singly protonated molecular ions for each alkaloid and methysergide (internal standard), were detected by single-ion monitoring (SIM). Calibration curves were obtained over a linear range of 0.1 to 40 pmol on column with correlation coefficients better than 0.994, Method recoveries were 68.4% to 111.0%. Intra-assay precision was 3.4% to 16.1%. Matrix effects were observed and overcome by introducing matrix components into calibrant solutions to create matrix-diluted standards. Limits of detection and quantitation were 0.05 pmol and 0.1 pmol, respectively. Method ruggedness tests resulted in recoveries of 86.1 to 122% with an interassay precision of 7.9% to 22.8%. These results indicate that this method is suitable for quantitation of alkaloids extracted from in vitro-exposed vascular tissue.
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