Premium
Development of a liquid chromatography/tandem mass spectrometry method for the quantification of fumonisin B 1 , B 2 and B 3 in cornflakes
Author(s) -
Paepens C.,
De Saeger S.,
Van Poucke C.,
Dumoulin F.,
Van Calenbergh S.,
Van Peteghem C.
Publication year - 2005
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.2022
Subject(s) - chemistry , chromatography , mass spectrometry , tandem mass spectrometry , tandem , analytical chemistry (journal) , materials science , composite material
A liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for the determination of fumonisin B 1 (FB 1 ), B 2 (FB 2 ) and B 3 (FB 3 ) in cornflakes is described. During method development, special attention was paid to the selection of a suitable internal standard (IS) in order to offer a good alternative for deuterated FB 1 . In this respect, the C 12 ‐sphinganine analogue (2 S ,3 R )‐2‐aminododecane‐1,3‐diol was chosen because of its structural similarity to the fumonisin backbone and its chromatographic elution between the target analytes. For the extraction of the fumonisins from the cornflakes matrix, MeOH/H 2 O (adjusted to pH 4 with 0.1 M HCl; 70:30, v/v), ACN/MeOH/H 2 O (25:25:50, v/v/v) and acidified ACN/MeOH/H 2 O (25:25:50, v/v/v; pH 4) were evaluated. Preference was given to acidified MeOH/H 2 O (70:30, v/v) with mean recoveries (n = 12) for FB 1 , FB 2 and FB 3 of, respectively, 84 ± 10, 78 ± 7 and 85 ± 9%. Cleanup was performed using immunoaffinity columns (FumoniTest®, VICAM). The chromatography was performed under isocratic conditions at a flow of 0.3 mL min −1 with a mobile phase consisting of ACN/H 2 O (60:40, v/v) containing 0.3% formic acid. The mass spectrometer was operated in the positive electrospray ionization (ESI+) mode using multiple reaction monitoring (MRM). An intralaboratory validation was conducted with fortified samples determining limits of detection (LOD), limits of quantification (LOQ), precision, trueness, specificity and measurement uncertainty. The LOD concentrations for FB 1 , FB 2 and FB 3 were 20, 7.5 and 12.5 µg/kg. The LOQs were 40 µg/kg for FB 1 , 15 µg/kg for FB 2 and 25 µg/kg for FB 3 . The coefficients of variation (CVs) under repeatability conditions varied from 11 to 13% for FB 1 , from 9 to 14% for FB 2 and from 7 to 10% for FB 3 . Under within‐laboratory reproducibility conditions, the CVs ranged from 12 to 17% for FB 1 , from 9 to 16% for FB 2 and from 7 to 13% for FB 3 . The percent bias for FB 1 varied from −12 to −10%, while for FB 2 and FB 3 bias ranged, respectively, from −4 to −2% and from −12 to −5%. The expanded measurement uncertainties for FB 1 , FB 2 and FB 3 were, respectively, 19, 18 and 22%. Copyright © 2005 John Wiley & Sons, Ltd.