A novel quantification method for sulfur-containing biomarkers of formaldehyde and acetaldehyde exposure in human urine
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RESEARCH PAPER
A novel quantification method for sulfur-containing biomarkers of formaldehyde and acetaldehyde exposure in human urine and plasma samples Anne Landmesser 1,2 & Gerhard Scherer 1 & Nikola Pluym 1 & Reinhard Niessner 2 & Max Scherer 1 Received: 3 June 2020 / Revised: 23 July 2020 / Accepted: 14 August 2020 # Springer-Verlag GmbH Germany, part of Springer Nature 2020
Abstract A novel method for the quantification of the sulfur-containing metabolites of formaldehyde (thiazolidine carboxylic acid (TCA) and thiazolidine carbonyl glycine (TCG)) and acetaldehyde (methyl thiazolidine carboxylic acid (MTCA) and methyl thiazolidine carbonyl glycine (MTCG)) was developed and validated for human urine and plasma samples. Targeting the sulfur-containing metabolites of formaldehyde and acetaldehyde in contrast to the commonly used biomarkers formate and acetate overcomes the high intra- and inter-individual variance. Due to their involvement in various endogenous processes, formate and acetate lack the required specificity for assessing the exposure to formaldehyde and acetaldehyde, respectively. Validation was successfully performed according to FDA’s Guideline for Bioanalytical Method Validation (2018), showing excellent performance with regard to accuracy, precision, and limits of quantification (LLOQ). TCA, TCG, and MTCG proved to be stable under all investigated conditions, whereas MTCA showed a depletion after 21 months. The method was applied to a set of pilot samples derived from smokers who consumed unfiltered cigarettes spiked with 13C-labeled propylene glycol and 13Clabeled glycerol. These compounds were used as potential precursors for the formation of 13C-formaldehyde and 13C-acetaldehyde during combustion. Plasma concentrations were significantly lower as compared to urine, suggesting urine as suitable matrix for a biomonitoring. A smoking-related increase of unlabeled biomarker concentrations could not be shown due to the ubiquitous distribution in the environment. While the metabolites of 13C-acetaldehyde were not detected, the described method allowed for the quantification of 13C-formaldehyde uptake from cigarette smoking by targeting the biomarkers 13C-TCA and 13 C-TCG in urine.
Keywords Formaldehyde . Acetaldehyde . LC-MS/MS . Stable labeled isotopes . Biomarkers Abbreviations AA Acetaldehyde FA Formaldehyde TCA Thiazolidine carboxylic acid TCG Thiazolidine carbonyl glycine MTCA Methyl thiazolidine carboxylic acid Electronic supplementary material The online version of this article (https://doi.org/10.1007/s00216-020-02888-y) contains supplementary material, which is available to authorized users. * Max Scherer [email protected] 1
ABF Analytisch-Biologisches Forschungslabor GmbH, Semmelweisstrasse 5, 82152 Planegg, Germany
2
Chair for Analytical Chemistry, Technische Universität München, Marchioninistraße, 81377 Munich, Germany
MTCG PCF
Methyl thiazolidine carbonyl glycine Propyl chloroformate
Introduction Formaldehyde (FA) is classified as carcinogenic to humans (group 1) and ac
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