Abstract
Ergot sclerotia effect cereal crops intended for consumption. Ergot alkaloids within ergot sclerotia are assessed to ensure contamination is below safety standards established for human and animal health. Ergot alkaloids exist in two configurations, the R and S-epimers. It is important to quantify both configurations. The objective of this study was to validate a new ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method for quantification of six R and six S-epimers of ergot alkaloids in hard red spring wheat utilizing deuterated lysergic acid diethylamide (LSD-D3) as an internal standard. Validation parameters such as linearity, limit of detection (LOD), limit of quantification (LOQ), matrix effects, recovery and precision were investigated. For the 12 epimers analyzed, low LOD and LOQ values were observed, allowing for the sensitive detection of ergot epimers. Matrix effects ranged between 101–113% in a representative wheat matrix. Recovery was 68.3–119.1% with an inter-day precision of <24% relative standard deviation (RSD). The validation parameters conform with previous studies and exhibit differences between the R and S-epimers which has been rarely documented. This new sensitive method allows for the use of a new internal standard and can be incorporated and applied to research or diagnostic laboratories.
Highlights
Mycotoxins continue to be a concern for the safety and quality of food and feed [1,2]
The objective of this study was to validate a new method for the simultaneous detection and quantification of R and S-epimers of ergot alkaloids utilizing deuterated lysergic acid diethylamide (LSD-D3) as a new internal standard
The instrumental limit of detection (LOD) ranged from 0.00893–0.225 μg/kg and the instrumental limit of quantification (LOQ) ranged from 0.0295–0.744 μg/kg for all 12 ergot epimers (Table 1)
Summary
Mycotoxins continue to be a concern for the safety and quality of food and feed [1,2]. The fungus Claviceps purpurea infects cereal crops forming visibly dark sclerotia that contain secondary metabolites known as ergot alkaloids [3]. Ergot alkaloids have two configurations known as the R-epimer and S-epimer. Rotation of a functional group on the chemical structure at the carbon-8 defines the epimer. Of the ergot alkaloids produced by Claviceps purpurea, six R and six corresponding S epimers are quantified in food and feed samples [7]. The corresponding S-epimers are ergocorninine, ergocristinine, ergocryptinine, ergometrinine, ergosinine and ergotaminine. Ergot epimers have different concentrations within the sclerotia depending on the geographic location and crop type [9]
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