Talanta paper on the top-down evaluation of the measurement uncertainty from correlated validation data following regulated validation design.
Link: https://www.sciencedirect.com/science/article/abs/pii/S0039914020306779
#Metrology #Uncertainty #Validation #AnalyticalChemistry #Crossvalidation #Correlation
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This work presents and cross-validates a novel top-down measurement uncertainty evaluation adapted to a common method validation design for the quantification of an impurity in active pharmaceutical ingredients, API. This methodology was successfully applied to the quantification of Pd in an intermediate of an API (iAPI) by ICP-MS after sample digestion, where method validation followed ICH and USP guidelines.
The method validation involved the replicate analysis of an iAPI with native analyte concentration before and after spiking at three different concentration levels by two analysts in two days. The uncertainty quantification considered the correlation between uncertainty components from tests performed on the same day and/or by using the same standard. The uncertainty model was cross-validated by randomly transferring some experimental data from method validation to analysis quality control. The measurement uncertainty was used to quantify the risk of a false acceptance of an iAPI. This work also describes the first evaluation of the uncertainty of elemental impurities quantification in pharmaceutical products.