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Harmonized Quality Assurance/Quality Control Provisions for Nontargeted Measurement of Urinary Pesticide Biomarkers in the HBM4EU Multisite SPECIMEn Study

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VITALE Chiara Maria LOMMEN Arjen HUBER Carolin WAGNER Kevin BORJA Garlito Molina NIJSSEN Rosalie PRICE Elliott James BLOKLAND Marco FREDERIKE van Tricht MOL Hans G J KRAUSS Martin DEBRAUWER Laurent PARDO Olga LEON Nuria KLÁNOVÁ Jana ANTIGNAC Jean-Philippe

Year of publication 2022
Type Article in Periodical
Magazine / Source Analytical chemistry
MU Faculty or unit

Faculty of Science

Keywords Anatomy; Extraction; Mass spectrometry; Quality management; Solvents
Description A set of quality assurance/quality control (QA/QC) criteria for nontargeted measurement of pesticide exposure markers in a large-scale study of human urine has been proposed and applied across five laboratories within the HBM4EU project. Quality control material, including reference standards and fortified pooled urine samples (QC urine) were prepared in a centralized way and distributed across participants to monitor analytical performance and consistency of the liquid chromatography coupled to high-resolution mass spectrometry data generated with a harmonized workflow. Signal intensities, mass accuracy, and retention times of selected QA/QC markers covering a broad range of physicochemical properties were monitored across QC solvent standards, QC urine samples, study urine samples, and procedural blanks, setting acceptance thresholds for repeatability and accuracy. Overall, results showed high repeatability of the collected data. The RSDs of the signal intensities were typically below 20-30% in QC and study samples, with good stability of the chromatographic separation (retention time drift within 2-4 s intrabatch and 5 s interbatch) and excellent mass accuracy (average error < 2 ppm). The use of the proposed criteria allowed for the identification of handling errors, instrumental issues, and potential batch effects. This is the first elaboration of harmonized QA/QC criteria applied across multiple laboratories to assess the quality of data generated by nontargeted analysis of human samples.
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