Abstract
The validation of analytical methods is of crucial importance in several fields of application. A new protocol for the validation of chromatographic methods has been proposed. The overall protocol is described in a parallel paper, where the case of a multi-targeted gas chromatography – mass spectrometry (GC–MS) method for the determination of androgens in human urine is in-depth discussed. The purpose of this paper is to report the details about the GC–MS separation and detection of the target analytes, and to provide the mathematical formulas needed to perform the validation of the principal parameters. Briefly, the validation protocol foresees the repetition of three calibration curves in three different days, providing a total amount of nine replicates. Such a structured design allows to use the same experiments to•perform a rigorous calibration study, by the evaluation of heteroscedasticity, comparison of several weights and linear/quadratic calibration curves.•determine several parameters which are traditionally computed from dedicated experiments, namely intra- and inter-day accuracy and precision, limit of detection, specificity, selectivity, ion abundance repeatability, and carry over.•Finally, few further experiments are necessary to evaluate the retention time repeatability, matrix effect and extraction recovery.
Highlights
Method ArticleEugenio Alladio a,b,1, Eleonora Amante a,b,1,∗, Cristina Bozzolino a, Fabrizio Seganti b, Alberto Salomone a,b, Marco Vincenti a,b, Brigitte Desharnais c a Dipartimento di Chimica, Università degli Studi di Torino, Turin, Italy b Centro Regionale Antidoping e di Tossicologia “A. Bertinaria”, Orbassano (Turin), Italy c Laboratoire de sciences judiciaires et de médecine légale, Montreal, Quebec, Canada abstract
The details related to the separation and acquisition methods are reported in this paper; the oven temperature program of the gas chromatograph is reported in Fig. 1, together with the typical total ion current (TIC) profile of a real urine sample
Limit of detection (LOD) The limit of detection is the lower concentration detectable with the specified analytical method. It can be evaluate using several different approaches; here, we propose the Hubaux and Vos’ computation [7]
Summary
Eugenio Alladio a,b,1, Eleonora Amante a,b,1,∗, Cristina Bozzolino a, Fabrizio Seganti b, Alberto Salomone a,b, Marco Vincenti a,b, Brigitte Desharnais c a Dipartimento di Chimica, Università degli Studi di Torino, Turin, Italy b Centro Regionale Antidoping e di Tossicologia “A. Bertinaria”, Orbassano (Turin), Italy c Laboratoire de sciences judiciaires et de médecine légale, Montreal, Quebec, Canada abstract. Eugenio Alladio a,b,1, Eleonora Amante a,b,1,∗, Cristina Bozzolino a, Fabrizio Seganti b, Alberto Salomone a,b, Marco Vincenti a,b, Brigitte Desharnais c a Dipartimento di Chimica, Università degli Studi di Torino, Turin, Italy b Centro Regionale Antidoping e di Tossicologia “A. The validation protocol foresees the repetition of three calibration curves in three different days, providing a total amount of nine replicates. Such a structured design allows to use the same experiments to. Method name: Effective validation protocol for chromatography mass spectrometry analytical methods Keywords: Chromatographic method, Validation protocol, Multiresidual analysis, GC-MS Article history: Received 9 April 2020; Accepted 6 May 2020; Available online 16 May 2020. Subject area: More specific subject area: Method name: Name and reference of original method: Resource availability: Chemistry Analytical Chemistry Effective validation protocol for chromatography – mass spectrometry analytical methods Not applicable Not applicable
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