Jm. Bosque-sendra et al., Decision protocol for checking robustness with previous outlier detection in the validation of analytical methods, FRESEN J AN, 365(6), 1999, pp. 480-488
A general procedure based on variation of experimental design for checking
robustness in the validation of analytical methods is presented. This proce
dure, which is easy to apply, consists in estimating the main total effects
, in detecting outliers, checking the curvature and in determining the main
side effects. Two methodologies based on the analysis of a) the residuals
from the reduced model and b) the replicates from the reconstructed design
were employed for the detection of outliers. In further studies, general ex
perimental design principles were applied using two- and three-level factor
ial designs. In some cases, a dummy variable was introduced in order not to
modify the structure of the designs utilized.