Effective validation of chromatographic analytical methods: The illustrative case of androgenic steroids.

Effective validation of chromatographic analytical methods: The illustrative case of androgenic steroids. Talanta. 2020 Aug 01;215:120867 Authors: Alladio E, Amante E, Bozzolino C, Seganti F, Salomone A, Vincenti M, Desharnais B Abstract The increasing need to develop quantitative chromatographic methods with upgradable multi-targeted approach, allowing flexible and reliable application on large daily workload makes the implementation of an efficient strategy of method's validation and maintenance crucial for the quality assurance policy. The expounding case of a gas chromatographic-mass spectrometric method for the urinary endogenous steroid profiling is presented to illustrate a validation strategy that combines rigorous estimation of validation parameters with highly efficient use of the collected data. The analysis of blank urine samples fortified at six concentration levels with 18 targeted steroids was replicated nine times in three working sessions along twelve days. This dataset of 54 analysis formed the groundwork on which the statistical evaluation of several validation parameters was founded, including calibration, intra- and inter-day accuracy and precision, limit of detection (LOD), limit of quantification, ion abundance ratio repeatability, selectivity, specificity, and carry-over. The preliminary comparison of the response variances at different concentration levels provided the evaluation for heteroscedasticity. Then,...
Source: Talanta - Category: Chemistry Authors: Tags: Talanta Source Type: research