Development of a gas chromatography/mass spectrometry method to quantify several urinary monohydroxy metabolites of polycyclic aromatic hydrocarbons in occupationally exposed subjects

• Published in: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Vol. 875; no. 2; pp. 531 - 540
• Main Authors: Campo, Laura, Rossella, Federica, Fustinoni, Silvia
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 15.11.2008; Elsevier
• Subjects: Analysis; Analytical, structural and metabolic biochemistry; Biological and medical sciences; Biological monitoring; Chrysenes - metabolism; Chrysenes - urine; Drug Stability; Environmental Monitoring - methods; Fluorenes - metabolism; Fluorenes - urine; Fundamental and applied biological sciences. Psychology; Gas Chromatography-Mass Spectrometry - methods; GC/MS; General pharmacology; Humans; Linear Models; Male; Medical sciences; Naphthols - metabolism; Naphthols - urine; Occupational Exposure - analysis; Pharmacology. Drug treatments; Phenanthrenes - metabolism; Phenanthrenes - urine; Polycyclic aromatic hydrocarbons; Polycyclic Aromatic Hydrocarbons - metabolism; Polycyclic Aromatic Hydrocarbons - urine; Pyrenes - analysis; Pyrenes - metabolism; Reference Standards; Reproducibility of Results; Sensitivity and Specificity; Urinary metabolites; Urinary metabolites; Polycyclic aromatic hydrocarbons; GC/MS; Biological monitoring; Human; Urine; Hydrocarbon; Metabolite; Polycyclic aromatic compound; Occupational exposure; Development; Mass spectrometry; Quantitative analysis
• ISSN: 1570-0232; 1873-376X
• DOI: 10.1016/j.jchromb.2008.10.017

The aim of this study was the development of a method for the determination of 12 urinary monohydroxy metabolites of PAHs, namely 1-hydroxynaphthalene, 2-hydroxynaphthalene, 2-hydroxyfluorene, 9-hydroxyfluorene, 1-hydroxyphenanthrene, 2-hydroxyphenanthrene, 3-hydroxyphenanthrene, 4-hydroxyphenanthrene, 9-hydroxyphenanthrene, 1-hydroxypyrene, 6-hydroxychrysene, and 3-hydroxybenzo[ a]pyrene. Analytes were determined in the presence of deuterated analogues as internal standards, by GC/MS operating in the electron impact mode. Sample preparation was performed by enzymatic hydrolysis of glucoronate and sulphate conjugates of hydroxy metabolites of PAHs, liquid–liquid extraction with n-hexane, and derivatization with a silylating reagent. The method is very specific, limits of quantification are in the range 0.1–1.4 μg/l, and range of linearity is from limit of detection to 208 μg/l. Within- and between-run precision, expressed as coefficient of variation, are <20%; accuracy for most analytes is within 20% of the theoretical value. An application of the proposed method to the analysis of 10 urine samples from coke-oven workers shows that 1-hydroxynaphthalene and 2-hydroxyfluorene were the most abundant compounds (median 61.4 and 69.7 μg/l, respectively), while 6-hydroxychrysene, and 3-hydroxybenzo[ a]pyrene were always below the quantification limit.