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ARS Home » Northeast Area » Beltsville, Maryland (BHNRC) » Beltsville Human Nutrition Research Center » Food Composition and Methods Development Laboratory » Research » Publications at this Location » Publication #156068
Title: RAPID TCA EXTRATION/LC METHOD FOR THE DETERMINATION OF NICOTINAMIDE IN COMMERCIAL CEREALS

Author
item Lacroix, Denis
item Wolf, Wayne
item KWANSA, ALBERT - 1235-15-00

Submitted to: Cereal Chemistry
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: 1/30/2005
Publication Date: 2/28/2005
Citation: Lacroix, D.E., Wolf, W.R., Kwansa, A.L. 2005. Determination of nicotinamide in commercial cereals by tca extraction/liquid chromatography. Cereal Chemistry. 82(3):277-281.

Interpretive Summary: A liquid chromatographic (LC) method has been modified for the determination of fortified nicotinamide in reference and commercial cereal products. Unbound nicotinamide in fortified cereal is extracted with trichloroacetic acid, and chromatographed on a reversed phase column using a mobile phase of methanol/water) with sodium dioctylsulphosuccinate as the ion-pairing agent. Using Spectral Analysis software, a 3-dimensional view showed only nicotinamide under the LC peak. Nicotinamide recoveries for the reference cereals of VMA-195 and VMA 399 (from the AACC) and SRM-19-B (from General Mills) ranged from 90-103% of assigned value. Experimental values for oat, corn, rice, and bran commercial cereals ranged from 103%-170% of label value, showing that niacin content in commercial cereals may be significantly above declared label values, which is allowed to ensure compliance with shelf life. These data have implications in making precise estimates of niacin intake based upon label claims. These data will be used by food testing and analysis laboratories in the public and private sector and by nutrition scientists who are estimating dietary intake of niacin from food surveys.

Technical Abstract: A liquid chromatographic method of Woollard and Indyk has been adapted for the determination of fortified nicotinamide in reference samples and commercial cereal products. Unbound nicotinamide in fortified cereal is extracted with 0.6M trichloroacetic acid, and chromatographed on a C-18-RP column using a mobile phase of 75% methanol/water with an the ion-pairing agent. Using Spectral Analysis software, Similarity Index spectral matches of nicotinamide standard and the LC peak were near 100%, indicating the absence of interferences. Nicotinamide recoveries for the reference cereals of VMA-195 and VMA 399 (from the American Association of Cereal Chemists) and SRM-19-B (from General Mills) ranged from 90-103% of assigned value. Experimental values for oat, corn, rice, and bran commercial cereals ranged from 103%-170% of label value, showing that niacin content in commercial cereals may be significantly above declared label values. These levels are not surprising since manufacturers are allowed to fortify some nutrient supplements in foods at a level higher than the declared label level to ensure compliance with shelf life. These data show that estimates of niacin intake based upon label claims may be erroneous.