Andriy Tkachenko1, Kelly Benson2, Michelle Mostrom2, Jake Guag1, Renate Reimschuessel1, Brett Webb2.
Abstract
BACKGROUND: Ergot alkaloids are mycotoxins produced by the fungus Claviceps, which can contaminate grains and pose a health risk to humans and animals. Validation of an ergot alkaloid method in collaborative projects can be challenging due to instability of analytes, a lack of reliable reference materials, and a fully validated reference method.
OBJECTIVE: To extensively evaluate performance of a quantitative UHPLC-MS/MS method to detect ten ergot alkaloids at concentrations between 16 and 500 ng/g in grains.
METHOD: The method performance was evaluated in the Blinded Method Test (BMT) exercise, which allowed organizers to successfully address the challenges. Forty completely blinded test samples were prepared in an independent laboratory and shipped to a participating laboratory to analyze on two separate days.
RESULTS: Precision, accuracy, and HorRatr values met or exceeded the U.S. Food and Drug Administration recommendations. The design of the BMT exercise provided a high degree of confidence in data and conclusions drawn.
CONCLUSIONS: The method performed in a manner as expected, and the method can be used by the laboratory for routine testing of wheat and rye grains. HIGHLIGHTS: BMT of laboratory methods facilitate validation of tests by evaluating performance in an unbiased manner. © AOAC INTERNATIONAL 2021. All rights reserved. For permissions, please email: journals.permissions@oup.com.
BACKGROUND: Ergot alkaloids are mycotoxins produced by the fungus Claviceps, which can contaminate grains and pose a health risk to humans and animals. Validation of an ergot alkaloid method in collaborative projects can be challenging due to instability of analytes, a lack of reliable reference materials, and a fully validated reference method.
OBJECTIVE: To extensively evaluate performance of a quantitative UHPLC-MS/MS method to detect ten ergot alkaloids at concentrations between 16 and 500 ng/g in grains.
METHOD: The method performance was evaluated in the Blinded Method Test (BMT) exercise, which allowed organizers to successfully address the challenges. Forty completely blinded test samples were prepared in an independent laboratory and shipped to a participating laboratory to analyze on two separate days.
RESULTS: Precision, accuracy, and HorRatr values met or exceeded the U.S. Food and Drug Administration recommendations. The design of the BMT exercise provided a high degree of confidence in data and conclusions drawn.
CONCLUSIONS: The method performed in a manner as expected, and the method can be used by the laboratory for routine testing of wheat and rye grains. HIGHLIGHTS: BMT of laboratory methods facilitate validation of tests by evaluating performance in an unbiased manner. © AOAC INTERNATIONAL 2021. All rights reserved. For permissions, please email: journals.permissions@oup.com.
Entities:
Year: 2021
PMID： 33394021 DOI： 10.1093/jaoacint/qsaa173
Source DB: PubMed Journal: J AOAC Int ISSN： 1060-3271 Impact factor: 1.913