Development of a highly efficient in-tube solid-phase microextraction system coupled with UHPLC-MS/MS for analyzing...

Area of Science:

• Environmental Chemistry
• Analytical Chemistry
• Toxicology

Background:

• Hydroxyl polycyclic aromatic hydrocarbons (OH-PAHs) are mutagenic and carcinogenic.
• Detecting trace levels (ng/g) of OH-PAHs in biological samples is analytically challenging.
• A sensitive method is needed for OH-PAH analysis in complex matrices like urine and blood.

Purpose of the Study:

• To develop a novel, sensitive, and effective method for determining trace OH-PAHs in biological samples.
• To utilize a macroporous in-tube solid-phase microextraction monolith for sample enrichment.
• To quantify specific OH-PAHs in human urine and mouse blood samples.

Main Methods:

• Preparation of a macroporous in-tube solid-phase microextraction monolith using a thiol-yne click reaction.
• Coupling in-tube solid-phase microextraction with ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS).
• Analysis of four OH-PAHs (2-hydroxyanthraquinone, 1-hydroxypyrene, 1,8-dihydroxyanthraquinone, 6-hydroxychrysene) in urine and blood samples.

Main Results:

• Achieved low detection limits ranging from 0.137-11.0 ng/L.
• Obtained satisfactory recoveries between 83.1-113% with relative standard deviations of 3.2-9.7%.
• Successfully determined OH-PAHs in urine samples from smokers and non-smokers, and in mouse blood samples.

Conclusions:

• The developed UHPLC-MS/MS method coupled with macroporous monolith in-tube solid-phase microextraction is highly efficient for trace OH-PAH determination.
• The macroporous monolith provides effective enrichment of OH-PAHs from complex biological matrices.
• This method offers a sensitive approach for monitoring exposure to these harmful compounds.