Development and validation of an extraction method using ultra-high performance liquid chromatography-tandem mass
Cristiane Rosa da Silva1, Cristina Tonial Simões1, Isadora Fabris Laber1
1Department of Preventive Veterinary Medicine, Laboratory of Mycotoxicological Analyses, Federal University of Santa Maria, 97105-970 Santa Maria, Rio Grande do Sul, Brazil.
Abstract:
Ergot alkaloids (EAs) are a group of mycotoxins that contaminate cereal crops, particularly rye, barley, and wheat. Given the extensive global production of wheat, developing accurate analytical methods for detecting and quantifying these toxic substances is essential to ensure food safety. Therefore, this study aimed to develop and validate a method for the analysis of ergosine, ergocornine, α-ergocryptine, ergotaminine, and ergocristine in wheat samples by ultra-high-performance liquid chromatography coupled with tandem mass spectrometry, utilizing solid-liquid extraction with acetonitrile and formic acid as extraction solvents. The method was validated for the five EAs, providing recoveries of 79-110 %, intra- and inter-day relative standard deviations of <20 %, and a quantification limit of 1 μg/kg for all analytes. Analysis of reference materials from FAPAS proficiency tests demonstrated the methodology's suitability for its intended purpose (z-scores <2).
