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
Jensen Cherewyk, Taylor Grusie-ogilvie, Barry Blakley, Ahmad Al-dissi
Toxins January 20, 2022 Peer reviewed DOI: 10.3390/toxins14010022 via DOAJ
Summary
A new method using ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) was validated for quantifying six R and six S-epimers of ergot alkaloids in hard red spring wheat. The method showed low limits of detection and quantification, with matrix effects ranging from 101–113% and recovery rates between 68.3–119.1%. This validation demonstrates significant differences between the R and S-epimers, which have been infrequently documented.
Study at a glance
| Population | hard red spring wheat |
|---|---|
| Key finding | The validated UHPLC-MS/MS method allows for sensitive detection of ergot alkaloid epimers in wheat. |
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.