Quantification of monohydroxy-PAH metabolites in urine by solid-phase extraction with isotope dilution-GC-MS.
For measurement of biomarkers from polycyclic aromatic hydrocarbon (PAH) exposure, an analytical method is described quantifying hydroxylated PAH (OH-PAH) in urine samples. This method determined monohydroxy metabolites of naphthalene, fluorene, phenanthrene, fluoranthene, pyrene, chrysene, benzo[c]phenanthrene, and benz[a]anthracene. The sample preparation consisted of enzymatic hydrolysis, solid-phase extraction and derivatization with a silylating reagent. Five carbon-13 labeled standards were used for isotope dilution. Analytes were separated by gas chromatography (GC) and quantified with high-resolution mass spectrometry (HRMS). This method produced good recoveries (41-70%), linearity, and specificity. Data were corrected for blank levels from the naphthalene, fluorene, and phenanthrene metabolites. Method detection limits ranged from 2 ng L(-1) for 1-hydroxypyrene to 43.5 ng L(-1) for 1-hydroxynaphthalene. Using quality control charts from two urine pools, the method can be readily applied to biomonitoring PAH exposure.
Smith
Christopher J
CJ
Centers for Disease Control and Prevention, Atlanta, GA 30341, USA. cps6@cdc.gov
Huang
Wenlin
W
Walcott
Charisse J
CJ
Turner
Wayman
W
Grainger
James
J
Patterson
Donald G
DG
D002851:Chromatography, High Pressure Liquid; D004784:Environmental Monitoring / Q000379:methods; D005449:Fluorenes / Q000032:analysis; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D006801:Humans; D006868:Hydrolysis; D007553:Isotope Labeling / Q000379:methods; D013058:Mass Spectrometry / Q000379:methods; D009281:Naphthalenes / Q000032:analysis; D016273:Occupational Exposure; D010616:Phenanthrenes / Q000032:analysis; D011084:Polycyclic Aromatic Hydrocarbons / Q000652:urine*; D011721:Pyrenes / Q000032:analysis; D012015:Reference Standards; D013997:Time Factors
D005449:Fluorenes; D009281:Naphthalenes; D010616:Phenanthrenes; D011084:Polycyclic Aromatic Hydrocarbons; D011721:Pyrenes; C031721:naphthalene; C041509:fluorene; C031181:phenanthrene; C033146:1-hydroxypyrene