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http://dx.doi.org/10.13103/JFHS.2019.34.2.158

Development of Analytical Method for Ergot Alkaloids in Foods Using Liquid Chromatoraphy-Tandem Mass Spectrometry  

Chun, So Young (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
Chong, Euna (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
Lee, Bomnae (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
Kwon, Jin-Wook (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
Park, Hye Young (Herbal Medicine Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food Drug Safety)
Kim, Sheenhee (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
Gang, Giljin (Food Contaminants Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
Publication Information
Journal of Food Hygiene and Safety / v.34, no.2, 2019 , pp. 158-169 More about this Journal
Abstract
Ergot alkaloids are mycotoxin produced by fungi of the Claviceps genus, mainly by Claviceps purpurea in EU. Recently obtained informations indicates necessity for control the ergot in imported grains. Recent occurrence data of ergot alkaloids from EU countries indicate the necessities of management and control these toxins from the imported grains like rye, wheat, oat etc. The aim of this study is to optimize the liquid chromatography-tandem mass spectrometry method for determination of ergot alkaloids (ergometrine, ergosine, ergotamine, ergocornine, ergocryptine, ergocristine and their epimers (-inines) from grain and grain-based food. The test method was optimized by extracting the sample with acetonitrile containing 2 mM ammonium carbonate, purification with Mycosep cartridge, and instrumental analysis by LC-MS/MS using Syncronis C18 column. The standard calibration curves showed linearity with correlation coefficents; $R^2$ >0.99. Mean recoveries ranged from 72.0 to 111.3% at three different fortified levels (20, 50, and $100{\mu}g/kg$). The correlation coefficient expressed as precision was within the range of 1.9-12.9%. The limit or quantifications (LOQ) ranged from 0.012 to $0.058{\mu}g/kg$. The developed analytical method met the criteria of AOAC Int. and CAC validation parameters like accuracy and sensitivity. As a result, it was confirmed that the test method developed in this study is suitable for the simultaneous analysis of six species of ergot alkaloid from grains and grain products.
Keywords
Ergot alkaloid; Analytical method; Cereal products; LC-MS/MS;
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