Bottom-up uncertainty evaluation of complex measurements from correlated performance data: Determination of total Cr in yeast by ICP-MS after acid digestion

• Published in: Food chemistry Vol. 404; p. 134466
• Main Authors: Pluháček, Tomáš, Pechancová, Radka, Milde, David, Bettencourt da Silva, Ricardo J.N.
• Format: Journal Article
• Language: English
• Published: Elsevier Ltd 15.03.2023
• Subjects: Bottom-up evaluation; Correlated data; ICP-MS; Measurement uncertainty; Microwave digestion; Correlated data; Microwave digestion; ICP-MS; Measurement uncertainty; Bottom-up evaluation
• ISSN: 0308-8146; 1873-7072
• DOI: 10.1016/j.foodchem.2022.134466

[Display omitted] •Analyte recovery assessed from spiked yeast and certified reference material analyses.•Estimated recovery correlated from quantifications based on same ICP-MS calibration.•Mean recovery uncertainty from correlated data and between yeast recovery variability.•Uncertainty models of measurement from replicate digestion and analysis developed.•ICP-MS method with sample digestion fully validated following strict criteria. The objective interpretation of a measurement result requires knowing the associated uncertainty. The cost-effective collection of measurement performance data on the same day produces correlated values that can affect measurement uncertainty evaluation. This work describes a novel methodology for the bottom-up evaluation of measurements based on complex sample pretreatment and the instrumental quantification of the prepared sample applicable to correlated inputs. The numerical Kragten method is used to combine the uncertainty components shared in various analyte recovery determinations. The developed methodology was applied to the determination of total chromium in yeast samples by ICP-MS after microwave-assisted acid digestion. The developed analysis of yeast samples is fit for monitoring the contamination of this product since it is associated with a relative expanded uncertainty, U’, lower than 20%, ranging from 8.4% to 10.0% in determinations of Cr between 0.125 mg/kg and 305.5 mg/kg. Duplicate analyses are adequate for reference materials production (U′ < 7%).