Determination of fumonisins B-1 and b2 in corn by liquid chromatography/mass spectrometry with immunoaffinity column cleanup: Single-laboratory method validation

Senyuva H. Z. , Ozcan S., Cimen D., Gilbert J.

JOURNAL OF AOAC INTERNATIONAL, vol.91, no.3, pp.598-606, 2008 (SCI-Expanded) identifier

  • Publication Type: Article / Article
  • Volume: 91 Issue: 3
  • Publication Date: 2008
  • Journal Indexes: Science Citation Index Expanded (SCI-EXPANDED), Scopus
  • Page Numbers: pp.598-606
  • Middle East Technical University Affiliated: Yes


A single-laboratory method validation was conducted to establish the effectiveness of an immunoaffinity column cleanup procedure followed by liquid chromatography/mass spectrometry (LC/MS) for the determination of fumonisins B-1 and B-2 (FB1 + FB2) in corn. The test portion is extracted with acetonitrile-methanol-water (25 + 25 + 50). The extract is filtered, diluted with phosphate-buffered saline solution, and applied to an immunoaffinity column. FB1 + FB2 are removed with methanol and directly determined by reversed-phase LC with MS detection using selected-ion monitoring of 2 characteristic ions in each case. Test portions of blank corn samples were spiked with a mixture of FB1 + FB2 to give total levels of 200 and 500 ng/g, respectively. Recoveries of both FB1 and FB2 from spiked samples averaged 90.4-101%. Based on results for spiked raw corn (triplicates at 2 levels), the relative standard deviation for repeatability ranged from 2.8 to 7.1%. The accuracy of the method was demonstrated by analysis of Food Analysis Performance Assessment Scheme (FAPAS (R)) test material. The method was also applied to a small survey of processed corn products such as corn chips, cornflakes, and popcorn.