A liquid chromatographic method for determination of fumonisin B1 (FB1) and B2 (FB2) in corn and corn flakes was subjected to a collaborative study involving 23 laboratories, in which 5 blind duplicate sample pairs of each matrix were analyzed to establish the accuracy, repeatability and reproducibility characteristics of the method. Concentrations in the corn samples ranged from <0.05 (blank) to 1.41 µg/g FB1 and from <0.05 to 0.56 µg/g FB2, while in the corn flake samples ranged from <0.05 to 1.05 µg/g FB1 and from <0.05 to 0.46 µg/g FB2. The method involved a double extraction with acetonitrile-methanol-water (25+25+50), a clean-up through immunoaffinity column and the end determination of fumonisins by LC after derivatization with o-phthaldialdehyde (OPA). Relative standard deviations for within-laboratory repeatability (RSDr) of corn analyses ranged from 19 to 24% for FB1 and from 19 to 27% for FB2; for corn flakes RSDr ranged from 9 to 21% for FB1 and from 8 to 22% for FB2. Relative standard deviation for between-laboratory reproducibility (RSDR) of corn analyses ranged from 22 to 28% for FB1 and from 22 to 30% for FB2; for corn flakes RSDR ranged from 27 to 32% for FB1 and from 26 to 35% for FB2. Mean recoveries of FB1 and FB2 from corn spiked with FB1 at 0.80 µg/g and with FB2 at 0.40 µg/g were 76 and 72%, respectively; for corn flakes spiked at the same levels recoveries were 110 and 97% for FB1 and FB2, respectively. HORRAT ratios in the analysis of corn materials ranged from 1.44 to 1.53 for FB1 and from 0.96 to 1.48 for FB2, whereas for corn flake materials they ranged from 1.60 to 1.82 for FB1 and from 1.39 to 1.68 for FB2.
Determination of fumonisin B1 and B2 in corn and corn flakes by high performance liquid chromatography and immunoaffinity column-cleanup: collaborative study
Visconti A;Solfrizzo M;De Girolamo A
2001
Abstract
A liquid chromatographic method for determination of fumonisin B1 (FB1) and B2 (FB2) in corn and corn flakes was subjected to a collaborative study involving 23 laboratories, in which 5 blind duplicate sample pairs of each matrix were analyzed to establish the accuracy, repeatability and reproducibility characteristics of the method. Concentrations in the corn samples ranged from <0.05 (blank) to 1.41 µg/g FB1 and from <0.05 to 0.56 µg/g FB2, while in the corn flake samples ranged from <0.05 to 1.05 µg/g FB1 and from <0.05 to 0.46 µg/g FB2. The method involved a double extraction with acetonitrile-methanol-water (25+25+50), a clean-up through immunoaffinity column and the end determination of fumonisins by LC after derivatization with o-phthaldialdehyde (OPA). Relative standard deviations for within-laboratory repeatability (RSDr) of corn analyses ranged from 19 to 24% for FB1 and from 19 to 27% for FB2; for corn flakes RSDr ranged from 9 to 21% for FB1 and from 8 to 22% for FB2. Relative standard deviation for between-laboratory reproducibility (RSDR) of corn analyses ranged from 22 to 28% for FB1 and from 22 to 30% for FB2; for corn flakes RSDR ranged from 27 to 32% for FB1 and from 26 to 35% for FB2. Mean recoveries of FB1 and FB2 from corn spiked with FB1 at 0.80 µg/g and with FB2 at 0.40 µg/g were 76 and 72%, respectively; for corn flakes spiked at the same levels recoveries were 110 and 97% for FB1 and FB2, respectively. HORRAT ratios in the analysis of corn materials ranged from 1.44 to 1.53 for FB1 and from 0.96 to 1.48 for FB2, whereas for corn flake materials they ranged from 1.60 to 1.82 for FB1 and from 1.39 to 1.68 for FB2.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
