In-house validation of liquid chromatography tandem mass spectrometry for determination of semicarbazide in eggs and stability of analyte in matrix

• Published in: Journal of Chromatography A Vol. 1216; no. 46; pp. 8187 - 8191
• Main Authors: Stastny, K., Frgalova, K., Hera, A., Vass, M., Franek, M.
• Format: Journal Article
• Language: English
• Published: Netherlands Elsevier B.V 13.11.2009; Amsterdam; New York: Elsevier
• Subjects: Animals; Chickens; Chromatography, Liquid - instrumentation; Chromatography, Liquid - methods; coccidiostats; drug residues; Egg; eggs; Eggs - analysis; food contamination; Food Contamination - analysis; food matrix; Incurred material; LC-MS/MS validation; liquid chromatography; mass spectrometry; Semicarbazide; Semicarbazides - analysis; Stability study; tandem mass spectrometry; Tandem Mass Spectrometry - instrumentation; Tandem Mass Spectrometry - methods; LC-MS/MS validation; Egg; Incurred material; Stability study; Semicarbazide
• ISSN: 0021-9673; 1873-3778
• DOI: 10.1016/j.chroma.2009.05.087

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