getpdf     https://doi.org/10.17113/ftb.53.01.15.3770

Application of Liquid Chromatography/Ion Trap Mass Spectrometry Technique to Determine
Ergot Alkaloids in Grain Products

Marcin Bryła*, Krystyna Szymczyk, Renata Jędrzejczak and Marek Roszko

Prof. Wacław Dąbrowski Institute of Agricultural and Food Biotechnology, Department of Food Analysis, Rakowiecka 36, PL-02-532 Warsaw, Poland



Article history
:
Received June 18, 2014
Accepted November 21, 2014


Key words:
liquid chromatography/ion trap mass spectrometry, ergot alkaloids, rye, cereals



Summary:
A liquid chromatography/ion trap mass spectrometry-based method to determine six ergot alkaloids and their isomers is presented. The samples were cleaned on neutral alumina-based solid-phase extraction cartridges. The following method parameters were obtained (depending on the analyte and spiking level): method recovery from 63.0 to 104.6 %, relative standard deviation below 18 %, linear range from 1 to 325 μg/kg, linear correlation coefficient not less than 0.98. The developed analytical procedure was applied to determine the levels of ergot alkaloids in 65 samples of selected rye-based food products (flour – 34 samples, bran – 12 samples, rye – 18 samples, fl akes – 1 sample). Measurable levels of alkaloids were found in majority of the analysed samples, particularly in rye flour. Additionally, alkaloids were determined in ergot sclerotia isolated from rye grains. Total content was nearly 0.01 % (97.9 mg/kg). However, the alkaloid profile was dominated by ergocristine at 45.6 % (44.7 mg/kg), an alkaloid not commonly found in the tested food products. Ergocorninine at 0.2 % (0.2 mg/kg) was the least abundant alkaloid.


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