title: Quantification of urinary mono-hydroxylated metabolites of polycyclic aromatic hydrocarbons by on-line solid phase extraction-high performance liquid chromatography-tandem mass spectrometry.
abstract: Human exposure to polycyclic aromatic hydrocarbons (PAHs) can be assessed through monitoring of urinary mono-hydroxylated PAHs (OH-PAHs). Gas chromatography (GC) has been widely used to separate OH-PAHs before quantification by mass spectrometry in biomonitoring studies. However, because GC requires derivatization, it can be time consuming. We developed an on-line solid phase extraction coupled to isotope dilution-high performance liquid chromatography-tandem mass spectrometry (on-line-SPE-HPLC-MS/MS) method for the quantification in urine of 1-OH-naphthalene, 2-OH-naphthalene, 2-OH-fluorene, 3-OH-fluorene, 1-OH-phenanthrene, the sum of 2-OH and 3-OH-phenanthrene, 4-OH-phenanthrene, and 1-OH-pyrene. The method, which employed a 96-well plate platform and on-line SPE, showed good sensitivity (i.e., limits of detection ranged from 0.007 to 0.09 ng/mL) and used only 100 μL of urine. Accuracy, calculated from the recovery percentage at three spiking levels, varied from 94 to 113 %, depending on the analyte. The inter- and intra-day precision, calculated from 20 repeated measurements of two quality control materials, varied from 5.2 to 16.7 %. Adequate method performance was also confirmed by acceptable recovery (83-102 %) of two NIST standard reference materials (3672 and 3673). This high-throughput on-line-SPE-HPLC-MS/MS method can be applied in large-scale epidemiological studies. Graphical abstract Example LC-MS chromatogram of urinary mono-hydroxylated PAH metabolites.
authors: Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, 4770 Buford Hwy, Mailstop F53, Atlanta, 30341, GA, USA. ywang6@cdc.gov.
authors: Yuesong
authors: Y
authors: Wang
authors: Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, 4770 Buford Hwy, Mailstop F53, Atlanta, 30341, GA, USA.
authors: Lei
authors: L
authors: Meng
authors: Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, 4770 Buford Hwy, Mailstop F53, Atlanta, 30341, GA, USA.
authors: Erin N
authors: EN
authors: Pittman
authors: Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, 4770 Buford Hwy, Mailstop F53, Atlanta, 30341, GA, USA.
authors: Alisha
authors: A
authors: Etheredge
authors: Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, 4770 Buford Hwy, Mailstop F53, Atlanta, 30341, GA, USA.
authors: Kendra
authors: K
authors: Hubbard
authors: Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, 4770 Buford Hwy, Mailstop F53, Atlanta, 30341, GA, USA.
authors: Debra A
authors: DA
authors: Trinidad
authors: Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, 4770 Buford Hwy, Mailstop F53, Atlanta, 30341, GA, USA.
authors: Kayoko
authors: K
authors: Kato
authors: Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, 4770 Buford Hwy, Mailstop F53, Atlanta, 30341, GA, USA.
authors: Xiaoyun
authors: X
authors: Ye
authors: Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, 4770 Buford Hwy, Mailstop F53, Atlanta, 30341, GA, USA.
authors: Antonia M
authors: AM
authors: Calafat
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006900:Hydroxylation; D057230:Limit of Detection; D011084:Polycyclic Aromatic Hydrocarbons / Q000652:urine*; D011786:Quality Control; D012015:Reference Standards; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D011084:Polycyclic Aromatic Hydrocarbons
keywords: Exposure; HPLC-MS/MS; OH-PAHs; Polycyclic aromatic hydrocarbons (PAHs); Urine