In-house validation and factorial effect analysis of a liquid chromatography–tandem mass spectrometry method for the determination of corticosteroids in bovine and porcine muscle tissue

摘要

A sensitive and robust liquid chromatography–tandem mass spectrometry method allowing the rapid screening and confirmation of ten synthetic corticosteroids in bovine and porcine muscle tissue was developed and validated. The validation was conducted according to Commission Decision 2002/657/EC, Sect. 3.1.3 (“Validation according to alternative models”), by applying a matrix-comprehensive in-house validation concept. The decision limit, detection capability, recovery, repeatability, within-laboratory-reproducibility and measurement uncertainty were calculated. Furthermore, a factorial effect analysis was conducted to identify factors that have a significant influence on the method. To this end, factors considered to be relevant for the method in routine analysis (e.g. operator, duration of storage of the extracts before measurement, different lots of the cartridges and different species) were systematically varied on two levels during the validation study. Subsequently, the extent to which these factors influence the measurement results of the individual analytes was examined.