Determination of Hydroxy Polycyclic Aromatic Hydrocarbons in Human Urine Using Automated Microextraction by Packed Sorbent and Gas Chromatography-Mass Spectrometry

Abstract

A fast methodology for the determination of monohydroxy polycyclic aromatic hydrocarbons in human urine using a fully automated microextraction by packed sorbent coupled to a gas chromatograph-mass spectrometer is reported. Sample preparation requires simple hydrolysis, centrifugation, filtration, and dilution. The method does not require a derivatization step prior to analysis with gas chromatography and allows the measurement of up to three samples per hour after hydrolysis. Quantitation is carried out by a one-point standard addition allowing the determination of 6 analytes with good limits of detection (10.1-39.6 ng L^-1 in water and 0.5-19.4 µg L^-1 in urine), accuracy (88-110%) and precision (2.1-23.4% in water and 5.1-19.0% in urine) values. This method has been successfully applied to the analysis of six urine samples (three from smoker and three from non-smoker subjects), finding significant differences between both types of samples. Results were similar to those found in the literature for similar samples, which proves the applicability of the methodology.

Keywords: gas chromatography–mass spectrometry; microextraction by packed sorbent; polycyclic aromatic hydrocarbon metabolites; underivatized analytes; urine samples.

Figure 1

Scheme of the MEPS steps for two consecutive samples.

Figure 2

Test of filter materials.

Figure 3

Optimization of MEPS elution solvent volume.

Figure 4

Chromatograms of UHQ-water spiked at the LOQ level in water (a), compared to a urine sample analyzed (S1), non-spiked (b) and spiked (c). 1= 1-NAP, 2 = 2-NAP, 3 = 1-ACE, 4 = 9-FLU, 5 = 2-FLU, 6 = 9-PHE.