Study of the Reproducibility Characteristics of a Liquid Chromatographic Method for the Determination of Fumonisins B1 and B2 in Corn: IUPAC Collaborative Study

Abstract

Abstract An interlaboratory study of the reproducibility characteristics of a liquid chromatographic method for the determination of fumonisins B1 and B2 in corn was conducted in 11 laboratories in the United States, South Africa, Italy, Japan, United Kingdom, and The Netherlands. Each laboratory was supplied with 12 coded, blind duplicates of 6 samples of naturally contaminated corn containing different amounts of fumonisins B1 and B2 . Samples are extracted with methanol-water (3 + 1), extracts are centrifuged, and supernatants are cleaned up on strong-anion-exchange cartridges, which were supplied to participants. Solutions are derivatized with o-phthaldialdehyde, and individual fumonisins are determined by reversed-phase liquid chromatography with fluorescence detection. Quantitation is by comparison with the supplied fumonisin standards. The within-laboratory repeatability was determined by statistical analysis of data after exclusion of outliers. Relative standard deviations for within-laboratory repeatability varied from 7.7 to 25.5% for fumonisin B1 at concentrations between 200 and 2000 ng/g and from 12.5 to 36.8% for fumonisin B2 at concentrations between 70 and 740 ng/g. Relative standard deviations for betweenlaboratory reproducibility varied from 18.0 to 26.7% for fumonisin B1 and from 28.0 to 45.6% for fumonisin B2 at the concentrations mentioned above. These measures of variability indicate that the method is suitable for adoption as an official method provided that the accuracy characteristics are verified collaboratively.