Determination of semicarbazide in fresh egg and whole egg powder by liquid chromatography/tandem mass spectrometry: interlaboratory validation study.
An interlaboratory validation study was conducted according to harmonized protocols to evaluate the effectiveness of a liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for the determination of semicarbazide (SEM) in fresh whole egg and in an industrially processed whole egg powder. The sample was extracted with hydrochloric acid and derivatized with 2-nitrobenzaldehyde, with 1,2-[(15)N2(13)C]SEM as the internal standard. The extract was neutralized and purified on a solid-phase extraction cartridge. SEM was determined by reversed-phase LC with detection by MS/MS. Five fresh egg samples, of which 3 were obtained from hens fed nitrofurazone (NFZ), one was spiked with SEM at 50 microg/kg and one was a blank sample, and 5 industrial whole egg powder samples, of which 3 were spiked with fresh whole egg from hens fed NFZ, one was spiked with SEM at 350 microg/kg, and one was a blank sample, were sent to 15 laboratories in 10 different European countries. Results were obtained from 12 participants. Average recoveries of SEM from the fresh egg and the egg powder samples were 105.3 and 121.3%, respectively. The relative standard deviation for repeatability (RSDr) ranged from 2.9 to 9.3%, and the relative standard deviation for reproducibility (RSDR) ranged from 22.5 to 38.1%. The method showed acceptable within- and between-laboratory precision for both matrixes, as evidenced by the HorRat values, at the target levels for the determination of SEM.
De la Calle
Maria Beatriz
MB
European Commission, Directorate General Joint Research Centre, Institute for Reference Materials and Measurements, B-2440 Geel, Belgium. maria.de-la-calle@ec.europa.eu
Szilagyi
Szilard
S
D002138:Calibration; D002851:Chromatography, High Pressure Liquid; D004531:Eggs / Q000032:analysis*; D007202:Indicators and Reagents; D013058:Mass Spectrometry; D012015:Reference Standards; D015203:Reproducibility of Results; D012663:Semicarbazides / Q000032:analysis*; D012996:Solutions; D013048:Specimen Handling
D007202:Indicators and Reagents; D012663:Semicarbazides; D012996:Solutions