Analysis of Fumagillin in Honey by LC-MS/MS

An LC/MS/MS method has been optimized and validated for the quantification and confirmation of fumagillin in honey. Fumagillin is isolated and concentrated by RP polymeric SPE. Final extracts are analyzed using electrospray ionization LC/MS/MS in positive mode with a formic acid and ammonium formate...

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Bibliographic Details
Published in:Journal of AOAC International 2013-05, Vol.96 (3), p.687-695
Main Authors: DMITROVIC, Jasna, DURDEN, David A
Format: Article
Language:English
Subjects:
Biological and medical sciences
Confectionery products and chocolate industries, honey
Food industries
Formic acid
Fundamental and applied biological sciences. Psychology
Honey
Ionization
Nitriles
Organic acids
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Summary:An LC/MS/MS method has been optimized and validated for the quantification and confirmation of fumagillin in honey. Fumagillin is isolated and concentrated by RP polymeric SPE. Final extracts are analyzed using electrospray ionization LC/MS/MS in positive mode with a formic acid and ammonium formate–acetonitrile mobile phase. Method uncertainty was determined using two analytical systems from different manufacturers. The validation of this LC/MS/MS method for the detection of fumagillin demonstrated overall recovery of 99.3%, precision of 5.9%, expanded uncertainty of 13.2%, and LOD of 0.368 μg/kg using an Agilent 6410 triple quadrupole system. Robustness testing showed that the method is robust against small changes in the method parameters. The method has been successfully applied to test 30 honey samples received as part of the Canadian Food Inspection Agency inspection program for the presence of fumagillin. It also was externally evaluated through proficiency testing and found to be fit-for-purpose.
ISSN:1060-3271
1944-7922
DOI:10.5740/jaoacint.12-174