In-house validation of liquid chromatography tandem mass spectrometry for determination of semicarbazide in eggs and stability of analyte in matrix.
An improved LC-MS/MS method for the determination of semicarbazide in whole egg is described. Waters OASIS-MCX cation exchange purification cartridges increased the sensitivity for analysis by LC-MS/MS. The validation study was carried out according to criteria and requirements of Commission Decision 2002/657/EC for confirmatory analysis and provided the data as follows: The correlation coefficient for the matrix calibration curve, in the range of 0-5 microg kg(-1), was r=0.9968. The detection capability and decision limit, measured according to ISO11843-2, were CCalpha=0.20 microg kg(-1) and CCbeta=0.25 microg kg(-1). Repeatability (CVSr) and within-laboratory reproducibility (CVSwr) determined for the concentration levels of 0.2, 0.5 and 1.0 microg kg(-1) SEM ranged from 11.9 to 5.7% and 11.8 to 6.3%, respectively. The validated method was applied to investigate SEM stability in incurred materials (egg homogenates) during long-term storage at -20 degrees C and 4 degrees C. The study proved by a two-sampling test that SEM at levels of 17. 7, 1.2, 10.6 and 0.47 microg kg(-1) was stable for up to 12 months.
Stastny
K
K
Institute for the State Control of Veterinary Biologicals and Medicaments, Hudcova 56a, 621 00 Brno, Czech Republic.
Frgalova
K
K
Hera
A
A
Vass
M
M
Franek
M
M
D000818:Animals; D002645:Chickens; D002853:Chromatography, Liquid / Q000295:instrumentation / Q000379:methods*; D004531:Eggs / Q000032:analysis*; D005506:Food Contamination / Q000032:analysis; D012663:Semicarbazides / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000295:instrumentation / Q000379:methods*
D012663:Semicarbazides; C010059:carbamylhydrazine