Extensive Evaluation via Blinded Testing of an UHPLC-MS/MS Method for Quantitation of Ten Ergot Alkaloids in Rye and Wheat Grains.


Journal

Journal of AOAC International
ISSN: 1944-7922
Titre abrégé: J AOAC Int
Pays: England
ID NLM: 9215446

Informations de publication

Date de publication:
12 Jun 2021
Historique:
received: 20 04 2020
revised: 09 12 2020
accepted: 09 12 2020
pubmed: 5 1 2021
medline: 29 6 2021
entrez: 4 1 2021
Statut: ppublish

Résumé

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. 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. 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. 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. 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. BMT of laboratory methods facilitate validation of tests by evaluating performance in an unbiased manner.

Sections du résumé

BACKGROUND 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 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 METHODS
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 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 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 CONCLUSIONS
BMT of laboratory methods facilitate validation of tests by evaluating performance in an unbiased manner.

Identifiants

pubmed: 33394021
pii: 6062393
doi: 10.1093/jaoacint/qsaa173
doi:

Substances chimiques

Ergot Alkaloids 0

Types de publication

Journal Article

Langues

eng

Sous-ensembles de citation

IM

Pagination

546-554

Informations de copyright

© AOAC INTERNATIONAL 2021. All rights reserved. For permissions, please email: journals.permissions@oup.com.

Auteurs

Andriy Tkachenko (A)

Center for Veterinary Medicine, United States Food and Drug Administration, 8401 Muirkirk Road, Laurel, MD 20708, USA.

Kelly Benson (K)

Veterinary Diagnostic Laboratory, North Dakota State University, 4035 19th Ave. N. Fargo, ND 58102, USA.

Michelle Mostrom (M)

Veterinary Diagnostic Laboratory, North Dakota State University, 4035 19th Ave. N. Fargo, ND 58102, USA.

Jake Guag (J)

Center for Veterinary Medicine, United States Food and Drug Administration, 8401 Muirkirk Road, Laurel, MD 20708, USA.

Renate Reimschuessel (R)

Center for Veterinary Medicine, United States Food and Drug Administration, 8401 Muirkirk Road, Laurel, MD 20708, USA.

Brett Webb (B)

Veterinary Diagnostic Laboratory, North Dakota State University, 4035 19th Ave. N. Fargo, ND 58102, USA.

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Classifications MeSH