Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry（UPLC-MS/MS）Analysis of Nine Ergot Alkaloids in Cereals and Their Contamination Analysis
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Abstract:
In this study, ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was used to establish a method for simultaneous determination of nine ergot alkaloids in cereals including dihydroergocristine, ergocornine, ergocorninine, ergocristine, ergocristinine, ergocryptine, ergocryptinine, ergosine, and ergotamine. The sample was extracted with an acetonitrile-water (84+16) solution, and the extract was purified with dispersive solid phase extraction agent (PSA). The UPLC-MS/MS analysis employed a C18 column for separation, and a mobile phase consisting of 0.1% formic acid aqueous solution and acetonitrile for gradient elution, along with external standards for quantification. The limit of detection (LOD) and limit of quantitation (LOQ) of ergot alkaloids were 5 μg/kg and 20 μg/kg, respectively. The recovery of ergot alkaloids was in the range of 50%~90% at the concentration of 45~75 μg/kg. At the same time, high-resolution mass spectrometry (HRMS) was used to determine the accurate mass and the secondary characteristic fragment ions of ergot alkaloids, to assist sample screening and confirmation. Twenty commercially available cereal samples were tested, with ergocristine and ergocristinine were detected in one sample and its content higher than the LOD but lower than the LOQ. This study provides a relatively effective detection method for ergot alkaloids in cereals and their products to ensure the safety of grains in China.
