Determination of dihydroergocryptine in human plasma and urine samples using on-line sample extraction?column-switching reversed-phase liquid chromatography?mass spectrometry

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

“…Different methods have been reported for the analysis of ergot alkaloids, including thin layer chromatography (TLC) (Salvat & Godoy, 2001), capillary electrophoresis (CE) (Franch & Blaschke, 1998), enzyme linked immunosorbent assay (ELISA) (Hill et al, 2001), gas chromatography (GC) with electron capture detection (ECD) (Barrow & Quigley, 1975), liquid chromatography (LC) with ultraviolet (Veress, 1993), fluorescence (Komarova & Tolkachev, 2001;Storm et al, 2008) or mass spectrometric (MS) (Burk et al, 2006;Kokkonen & Jestoi, 2010;Krska, Stubbings, Macarthur, & Crews, 2008;Mohamed, Gremaud, Rychoz-Payot, Tabet, & Guy, 2006) detection. In recent years, LC-MS has become the method of choice for mycotoxin determination (Shephard et al, 2011;Spanjer, 2010), and has provided an unequivocal identification of ergot alkaloids in various matrices (Friedrich et al, 2004;Lehner, Craig, Fannin, Bush, & Tobin, 2005;Mohamed et al, 2006). However, validated LC-MS methods for the simultaneous quantitative determination of the major ergot alkaloids in food and feed are scarce.…”

“…Such methods are required for the monitoring of these toxins, as well as for further research and study of the ergot problem. A number of the methods mentioned above have been used for biomedical application (Friedrich et al, 2004) and /or for identification purposes (Lehner et al, 2005). Some include no or only few -inine isomers (Burk et al, 2006;Kokkonen & Jestoi, 2010;Mohamed et al, 2006), possibly because of the lack of available standards.…”

Mass spectral characterization of ergot alkaloids by electrospray ionization, hydrogen/deuterium exchange, and multiple stage mass spectrometry: usefulness of precursor ion scan experiments

“…Thin‐layer chromatography (TLC),14, 15 high‐performance liquid chromatography (HPLC) with ultraviolet16, 17 or fluorimetric18, 19 detection, a gas liquid chromatography system (GLC) with electron capture detection,20, 21 and gas chromatography coupled to mass spectrometry (GC/MS)22, 23 have been reported for the determination of ergot alkaloids and lysergic acid derivatives. Several matrices were studied such as cereals and cereal products22, 24, 25 and human and animal biological fluids 15, 16, 21, 23, 26. However, TLC suffers from poor separation power and GC/MS has several drawbacks such as limited molecular weight range (ergot alkaloids have a molecular mass up to 609 Da), the need for compounds to be volatile or amenable to derivatization, a low loading capacity, and instability of some compounds towards heat.…”

“…However, TLC suffers from poor separation power and GC/MS has several drawbacks such as limited molecular weight range (ergot alkaloids have a molecular mass up to 609 Da), the need for compounds to be volatile or amenable to derivatization, a low loading capacity, and instability of some compounds towards heat. As an alternative, HPLC coupled to MS has provided an unequivocal identification of the alkaloids 26, 27. In a previous work, we have developed a liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI‐MS/MS) method to confirm and quantify the presence of five ergot alkaloids in rye flour samples 28…”