Validation of a New Sensitive Method for the Detection and Quantification of R and S-Epimers of Ergot Alkaloids in Canadian Spring Wheat Utilizing Deuterated Lysergic Acid Diethylamide as an Internal Standard

A new ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method was validated to quantify six R and six S-epimers of ergot alkaloids in hard red spring wheat, using deuterated lysergic acid diethylamide (LSD-D3) as an internal standard. The method showed low limits of detection and quantification, matrix effects between 101–113%, recovery of 68.3–119.1%, and inter-day precision below 24% relative standard deviation. These validation parameters align with previous studies and reveal differences between R and S-epimers that have rarely been documented. The sensitive method can be adopted by research or diagnostic laboratories.

Study at a glance

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.