title: Analysis of endogenous aldehydes in human urine by static headspace gas chromatography-mass spectrometry.
abstract: Endogenous aldehydes (EAs) generated during oxidative stress and cell processes are associated with many pathogenic and toxicogenic processes. The aim of this research was to develop a solvent-free and automated analytical method for the determination of EAs in human urine using a static headspace generator sampler coupled with gas chromatography-mass spectrometry (HS-GC-MS). Twelve significant EAs used as markers of different biochemical and physiological processes, namely short- and medium-chain alkanals, α,β-unsaturated aldehydes and dicarbonyl aldehydes have been selected as target analytes. Human urine samples (no dilution is required) were derivatized with O-2,3,4,5,6-pentafluorobenzylhydroxylamine in alkaline medium (hydrogen carbonate-carbonate buffer, pH 10.3). The HS-GC-MS method developed renders an efficient tool for the sensitive and precise determination of EAs in human urine with limits of detection from 1 to 15ng/L and relative standard deviations, (RSDs) from 6.0 to 7.9%. Average recoveries by enriching urine samples ranged between 92 and 95%. Aldehydes were readily determined at 0.005-50μg/L levels in human urine from healthy subjects, smokers and diabetic adults.
authors.affiliation: Department of Analytical Chemistry, Campus of Rabanales, University of Córdoba, E-14071 Córdoba, Spain.
authors.forename: María
authors.initials: M
authors.lastname: Serrano
authors.affiliation: Department of Analytical Chemistry, Campus of Rabanales, University of Córdoba, E-14071 Córdoba, Spain. Electronic address: qa1gafem@uco.es.
authors.forename: Mercedes
authors.initials: M
authors.lastname: Gallego
authors.affiliation: Department of Analytical Chemistry, Campus of Rabanales, University of Córdoba, E-14071 Córdoba, Spain.
authors.forename: Manuel
authors.initials: M
authors.lastname: Silva
mesh_terms: D000328:Adult; D000447:Aldehydes / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D012680:Sensitivity and Specificity; D012997:Solvents / Q000032:analysis; D016482:Urinalysis / Q000295:instrumentation* / Q000379:methods*
chemical_list: D000447:Aldehydes; D012997:Solvents
keywords: Endogenous aldehydes; Gas chromatography–mass spectrometry; Human urine; Oxidative stress; Static headspace technique