Title: Determination of Semicarbazide in Baby Food by Liquid Chromatography/Tandem Mass Spectrometry: Interlaboratory Validation Study
Citation: JOURNAL OF AOAC INTERNATIONAL vol. 89 no. 3 p. 728-734
Publication Year: 2006
JRC N°: JRC36279
URI: http://publications.jrc.ec.europa.eu/repository/handle/JRC36279
Type: Articles in periodicals and books
Abstract: An interlaboratory validation study funded by the European Commission, Directorate Generale for Health and Consumer Protection (DG SANCO), was conducted to evaluate the effectiveness of a liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for the determination of semicarbazide (SEM) in different types of baby food at a possible future European regulatory limit (10 ng/g). The test portion of the sample was extracted with hydrochloric acid, and the analyte was derivatized with 2-nitrobenzaldehyde, with 1,2(15N2, 13C) SEM as an internal standard. The extract was neutralized and then purified on a solid-phase extraction cartridge. The SEM was determined by reversed-phase LC with detection by MS/MS. Apple putee, rice pudding, and meat/vegetable meal baby food materials, spiked with SEM at levels of about 3,10, and 30 ng/g, respectively, were sent to 20 laboratories in 12 different European countries, which submitted results from 17 participants. Recoveries ranged from 88.8 to 106.1%. Based on results for spiked samples (blind pairs at 3 levels), the relative standard deviations for repeatability (RSDr) ranged from 4.2 to 6.9% and the relative standard deviations for reproducibility (RSD R) ranged from 16.6 to 24.3%. The method showed acceptable within- and between-laboratory precision for all 3 matrixes, as evidenced by HorRat values, at the target levels for the determination of SEM.
JRC Directorate:Health, Consumers and Reference Materials

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