Determination of fumonisins B1 and B2 in corn by liquid chromatography/mass spectrometry with immunoaffinity column cleanup: single-laboratory method validation.
A single-laboratory method validation was conducted to establish the effectiveness of an immunoaffinity column cleanup procedure followed by liquid chromatography/mass spectrometry (LCIMS) for the determination of fumonisins B1 and B2 (FBI + 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) test material. The method was also applied to a small survey of processed corn products such as corn chips, cornflakes, and popcorn.
TUBITAK, Ankara Test and Analysis Laboratory (ATAL), Konya Yolu No. 67, Besevler, 06530, Ankara, Turkey. hamide.senyuva@tubitak.gov.tr
Hamide Z
HZ
Senyuva
Sureyya
S
Ozcan
Dilek
D
Cimen
John
J
Gilbert
D002846:Chromatography, Affinity / Q000379:methods; D002853:Chromatography, Liquid / Q000379:methods* / Q000706:statistics & numerical data; D005506:Food Contamination / Q000032:analysis*; D037341:Fumonisins / Q000032:analysis* / Q000592:standards / Q000633:toxicity; D006801:Humans; D012015:Reference Standards; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods* / Q000706:statistics & numerical data; D003313:Zea mays / Q000737:chemistry* / Q000592:standards / Q000633:toxicity
D037341:Fumonisins; C056934:fumonisin B2; C056933:fumonisin B1