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  • A novel strategy for the determination of polycyclic aromatic hydrocarbon monohydroxylated metabolites in urine using ultra-high-performance liquid chromatography with tandem mass spectrometry.

A novel strategy for the determination of polycyclic aromatic hydrocarbon monohydroxylated metabolites in urine using ultra-high-performance liquid chromatography with tandem mass spectrometry.

Analytical and bioanalytical chemistry (2016-02-11)
Darina Lankova, Katerina Urbancova, Radim J Sram, Jana Hajslova, Jana Pulkrabova
ABSTRACT

In this study, a novel analytical approach for the determination of 11 monohydroxylated polycyclic aromatic hydrocarbon metabolites (OH-PAHs) in urine was developed and validated. The rapid, simple and high-throughput sample preparation procedure based on ethyl acetate extraction and subsequent purification by dispersive solid-phase extraction (d-SPE) employing a Z-Sep sorbent is used for the first time. For the identification/quantification of target compounds, ultra-high-performance liquid chromatography (U-HPLC) interfaced with tandem mass spectrometry (MS/MS) was applied. The results of validation experiments performed on the Standard Reference Material (SRM) 3673 (organic contaminants in non-smokers' urine) were in accordance with the certified values. The method recoveries ranged from 77 to 114 % with the relative standard deviation lower than 20 % and the quantification limits in the range of 0.010-0.025 ng mL(-1) (except for benzo[a]pyren-3-ol with 0.9 ng mL(-1)). Within the pilot study, the new method was used for the analysis of OH-PAHs in 50 urine samples. The concentrations of ΣOH-PAHs were in the range of 0.87-63 ng mL(-1) (1600-33,000 ng g(-1) creatinine), with naphthalen-2-ol (2-OH-NAP) and phenanthren-1-ol (1-OH-PHEN) being the most abundant exposure biomarkers detected in all samples.

MATERIALS
Product Number
Brand
Product Description

Supelco
Supel QuE, Z-Sep+ Bulk, pkg of 20 g
Supelco
Supel QuE, Z-Sep/C18 Tube, centrifuge tube volume 2 mL, pack of 100
Supelco
Supel QuE, Z-Sep Bulk
Supelco
Supel QuE, Z-Sep+ Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep+ Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep/C18 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible