Ergot alkaloids in rye flour determined by solid-phase cation-exchange and high-pressure liquid chromatography with fluorescence detection

Abstract

alkaloids in rye flour determined by solid phase cation-exchange and high pressure liquid chromatography with fluorescence detection. Food Additives and Contaminants, 2008, 25 (03) Ergot alkaloids (EAs) are mycotoxins which are undesirable contaminants of cereal products, particularly rye. A method was developed employing clean-up by cation-exchange solid phase extraction, separation by HPLC under alkaline conditions and fluorescence detection. It is capable of separating and quantifying both C8-isomers of ergocornine, a-ergocryptine, ergocristine, ergonovine, and ergotamine. The average recovery was 61±10 % with limits of detection from 0.2 to 1.1 µg kg-1. Therty-four unknown rye flour samples from Danish mills contained on average 46 µg kg-1 with a maximum content of 234 µg kg-1. The most common ergot alkaloids were ergotamine and a-ergocryptine including their C8-isomers. 54 % of the ergot alkaloids were detected as C(8)-S isomers.

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

“…After the infection is established, the fungus replaces the developing grain or seed with an alkaloid-containing hard black tuber-like wintering structure called sclerotium, also known as ergot or ergot body. The alkaloid pattern and individual alkaloid contents in sclerotia vary largely, due to differences in the maturity of the sclerotia and to other factors such as the fungal strain, the host plant, the geographical region and the prevailing weather conditions (Lombaert, 2001;Storm, Rasmussen, Strobel, & Hansen, 2008). Similarly, data from the literature indicate that the total alkaloid content in sclerotia can vary between 0.01% and 1% (w/w) (Burk, Hobel, & Richt, 2006;Lauber, Schnaufer, Gredziak, & Kiesswetter, 2005;Lombaert, 2001;Scott, 2009).…”

Development and Validation of an Analytical Method for Determination of Ergot Alkaloids in Animal Feedingstuffs with High Performance Liquid Chromatography-fluorescence Detection

“…For the separation of ergot alkaloids most authors used reverse phase C18 columns (Mohamed et al 2006, Storm et al 2008, Di Mavungu et al 2012 though, the separation was also performed on a C6 phenyl column (Muller et al 2009). As far as the mobile phase is concerned, the most popular composition was ammonium carbonate at different concentrations and acetonitrile (Storm et al 2008, Muller et al 2009, Bryła et al 2015 used in an isocratic and gradient mode as well.…”

“…As far as the mobile phase is concerned, the most popular composition was ammonium carbonate at different concentrations and acetonitrile (Storm et al 2008, Muller et al 2009, Bryła et al 2015 used in an isocratic and gradient mode as well. In the presented method the separation was also performed on a C18 column with the mobile phase consisted of ammonium carbonate and acetonitrile; however, a gradient mode was used which provided good separation of ergot alkaloids, and method selectivity.…”

An integrated targeted and untargeted approach for the analysis of ergot alkaloids in cereals using UHPLC – hybrid quadrupole time-of-flight mass spectrometry

“…Evaluation of the exposure and actual risk due to consumption of contaminated food and feedstuffs requires suitable analytical strategies. Analytical methods for the determination of ergot alkaloids include thin layer chromatography (TLC) (Salvat and Godoy, 2001), capillary electrophoresis (CE) (Franch and Blaschke, 1998), enzyme linked immunosorbent assay (ELISA) (Hill et al, 2001), gas chromatography (GC) with electron capture detection (ECD) (Barrow and Quigley, 1975), liquid chromatography (LC) with ultraviolet (Veress, 1993), fluorescence (Komarova and Tolkachev, 2001a;Storm et al, 2008) or mass spectrometric (MS) (Diana di Mavungu et al, 2012;Burk et al, 2006;Kokkonen and Jestoi, 2010;Krska et al, 2008a;Mohamed et al, 2006b) detection. Over the last decade, LC-MS has become a dominant tool for mycotoxin determination, and has provided an unequivocal identification of ergot alkaloids in various matrices (Diana di Mavungu et al, 2012;Friedrich et al, 2004;Kokkonen and Jestoi, 2009;Krska et al, 2008;Lehner et al, 2005;Mohamed et al, 2006a;Mohamed et al, 2006b).…”