Development and validation of a new LC–MS/MS method for the simultaneous determination of six major ergot alkaloids and their corresponding epimers. Application to some food and feed commodities

• Published in: Food chemistry Vol. 135; no. 1; pp. 292 - 303
• Main Authors: Diana Di Mavungu, José, Malysheva, Svetlana V., Sanders, Melanie, Larionova, Daria, Robbens, Johan, Dubruel, Peter, Van Peteghem, Carlos, De Saeger, Sarah
• Format: Journal Article
• Language: English
• Published: Kidlington Elsevier Ltd 01-11-2012; Elsevier
• Subjects: Biological and medical sciences; Cereal and baking product industries; Cereals; Ergot alkaloids; Feed; Feed and pet food industries; Food; Food industries; Fundamental and applied biological sciences. Psychology; LC–MS/MS; Validation; Validation; Cereals; Ergot alkaloids; LC–MS/MS; Food; Feed; LC-MS/MS; Alkaloid; Development; Cereal; Liquid chromatography; Method; Application
• ISSN: 0308-8146; 1873-7072
• DOI: 10.1016/j.foodchem.2012.04.098

► A Validated LC–MS/MS method for ergot alkaloids in food and feed is proposed. ► The method allows simultaneous determination of major ergot alkaloids and epimers. ► Stability of XBridge column under alkaline conditions allows improved chromatography. ► The sample preparation protocol allows minimising analyte epimerization. ► Ergot alkaloids were present (1–1145μg/kg) in Belgian food and feed commodities.
A liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated for the simultaneous determination of six major ergot alkaloids, ergometrine, ergosine, ergotamine, ergocornine, ergokryptine and ergocristine, as well as their corresponding epimers in food and feed samples. The method involves extraction under alkaline conditions and subsequent clean-up by applying a simple and rapid liquid–liquid partitioning procedure prior to LC–MS/MS analysis. Evaluation of the method revealed good linearity, accuracy and precision. The limits of quantification varied from 0.1 to 1μg/kg depending on the analyte and matrix. The average extraction and clean-up recoveries in different matrices were between 45 (only for ergometrine in biscuit) and 90%. The uncertainty associated with the analytical method was not higher than 51% and 30%, at concentration levels of 2.5 and 150μg/kg respectively. Analyte epimerization proved to be minimal during the analytical procedure. The method has been successfully applied to the determination of ergot alkaloids in some Belgian food and feed commodities. Ergot alkaloids were found in 104 out of 122 samples investigated. Ergosine was the most frequently occurring alkaloid, while the highest levels were observed for ergotamine, ergocristine or ergosine, depending on the product type. The total alkaloid content in positive samples varied from 1 to 1145μg/kg.