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 0–5μgkg−1, was r=0.9968. The detection capability and decision limit, measured according to ISO11843-2, were CCα=0.20μgkg−1 and CCβ=0.25μgkg−1. Repeatability (CVSr) and within-laboratory reproducibility (CVSwr) determined for the concentration levels of 0.2, 0.5 and 1.0μgkg−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°C and 4°C. The study proved by a two-sampling test that SEM at levels of 17. 7, 1.2, 10.6 and 0.47μgkg−1 was stable for up to 12 months.