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Determination of Semicarbazide in Baby Food by Liquid chromatography/tandem Mass Spectrometry: Interlaboratory Validation Study

Determination of Semicarbazide in Baby Food by Liquid chromatography/tandem Mass Spectrometry: Interlaboratory Validation Study

Richard Ginn, Lesley Wilson, Scheilla V C De Souza, Maria B de la Calle

J AOAC Int. May-Jun 2006;89(3):728-34.

PMID: 16792072

Abstract:

An interlaboratory validation study funded by the European Commission, Directorate General 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 puree, 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 (RSDR) 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.

Chemicals Related in the Paper:

Catalog Number	Product Name	Structure	CAS Number	Price
AS211236	2-Nitrobenzaldehyde semicarbazone-13C, 15N2			Price

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