Determination of Fumonisins B1 and B2 in Corn by Liquid Chromatography/Mass Spectrometry with Immunoaffinity Column Cleanup: Single-Laboratory Method Validation
Abstract: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 B1 and B2 (FB1+ FB2) in corn. The test portion is extracted with acetonitrilemethanolwater (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 90.4101. 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) test material. The method was also applied to a small survey of processed corn products such as corn chips, cornflakes, and popcorn.
Document Type: Research Article
Affiliations: 1: TUBITAK, Ankara Test and Analysis Laboratory (ATAL), Konya Yolu No. 67, Besevler, 06530, Ankara, Turkey. 2: Gazi University, Department of Chemistry, Besevler, 06500, Ankara, Turkey. 3: Central Science Laboratory, Food and Rural Affairs, Department for Environment, Sand Hutton, York, YO41 1LZ, United Kingdom.
Publication date: May 1, 2008
- The Journal of AOAC INTERNATIONAL publishes refereed papers and reviews in the fields of chemical, biological and toxicological analytical chemistry for the purpose of showcasing the most precise, accurate and sensitive methods for analysis of foods, food additives, supplements and contaminants, cosmetics, drugs, toxins, hazardous substances, pesticides, feeds, fertilizers and the environment available at that point in time. The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better methods of preparing samples for analysis; collaborative studies substantiating the performance of a given method; statistical techniques for evaluating data. The Journal will also publish other articles of general interest to its audience, e.g., technical communications; cautionary notes; comments on techniques, apparatus, and reagents.
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