Determination of the Main Ergot Alkaloids and Their Epimers in Oat-Based Functional Foods by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry

• Published in: Molecules (Basel, Switzerland) Vol. 26; no. 12; p. 3717
• Main Authors: Carbonell-Rozas, Laura, Gámiz-Gracia, Laura, Lara, Francisco J., García-Campaña, Ana M.
• Format: Journal Article
• Language: English
• Published: Basel MDPI AG 18.06.2021; MDPI
• Subjects: Acetonitrile; Alkaloids; Ammonium; Ammonium compounds; Calibration; Cereals; Chromatography; Dietary supplements; Ergot; ergot alkaloids; Ergotamine; Food contamination & poisoning; food supplements; Functional foods & nutraceuticals; High performance liquid chromatography; Liquid chromatography; Mass spectrometry; Mass spectroscopy; Mean square errors; oat; QuEChERS; Scientific imaging; Solid phases; Sorbents; Spectroscopy; UHPLC–MS/MS
• ISSN: 1420-3049; 1420-3049
• DOI: 10.3390/molecules26123717

An ultra-high performance liquid chromatography coupled to tandem mass spectrometry method is proposed for the determination of the major ergot alkaloids (ergometrine, ergosine, ergotamine, ergocornine, ergokryptine, ergocristine) and their epimers (ergometrinine, ergosinine, ergotaminine, ergocorninine, ergokryptinine, and ergocristinine) in oat-based foods and food supplements. A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure was applied as sample treatment, reducing the consumption of organic solvent and increasing sensitivity. This method involved an extraction with acetonitrile and ammonium carbonate (85:15, v/v) and a clean-up step based on dispersive solid-phase extraction, employing a mixture of C18/Z-Sep+ as sorbents. Procedural calibration curves were established and limits of quantification were below 3.2 μg/kg for the studied compounds. Repeatability and intermediate precision (expressed as RSD%) were lower than 6.3% and 15%, respectively, with recoveries ranging between 89.7% and 109%. The method was applied to oat-based products (bran, flakes, flour, grass, hydroalcoholic extracts, juices, and tablets), finding a positive sample of oat bran contaminated with ergometrine, ergosine, ergometrinine, and ergosinine (total content of 10.7 μg/kg).