Determination of semicarbazide in baby food by liquid chromatography/tandem mass spectrometry: interlaboratory validation study.
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.
Ginn
Richard
R
Central Science Laboratory (CSL), Sand Hutton, York, YO41 lLZ, United Kingdom.
Wilson
Lesley
L
De Souza
Scheilla V C
SV
de la Calle
Maria B
MB
D001547:Benzaldehydes / Q000032:analysis; D002138:Calibration; D002623:Chemistry Techniques, Analytical / Q000379:methods*; D002851:Chromatography, High Pressure Liquid; D002853:Chromatography, Liquid / Q000379:methods*; D005060:Europe; D005504:Food Analysis / Q000379:methods*; D006851:Hydrochloric Acid / Q000032:analysis; D007225:Infant Food; D013058:Mass Spectrometry / Q000379:methods*; D015203:Reproducibility of Results; D012663:Semicarbazides / Q000032:analysis* / Q000302:isolation & purification
D001547:Benzaldehydes; D012663:Semicarbazides; C010059:carbamylhydrazine; C043850:2-nitrobenzaldehyde; D006851:Hydrochloric Acid