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. 2018 Jul 26;23(8):1869.
doi: 10.3390/molecules23081869.

High-Throughput Analysis of Selected Urinary Hydroxy Polycyclic Aromatic Hydrocarbons by an Innovative Automated Solid-Phase Microextraction

Stefano Dugheri  1 , Alessandro Bonari  2 , Matteo Gentili  3 , Giovanni Cappelli  4 , Ilenia Pompilio  5 , Costanza Bossi  6 , Giulio Arcangeli  7 , Marcello Campagna  8 , Nicola Mucci  9
Affiliations

High-Throughput Analysis of Selected Urinary Hydroxy Polycyclic Aromatic Hydrocarbons by an Innovative Automated Solid-Phase Microextraction

Stefano Dugheri et al. Molecules. .

Abstract

High-throughput screening of samples is the strategy of choice to detect occupational exposure biomarkers, yet it requires a user-friendly apparatus that gives relatively prompt results while ensuring high degrees of selectivity, precision, accuracy and automation, particularly in the preparation process. Miniaturization has attracted much attention in analytical chemistry and has driven solvent and sample savings as easier automation, the latter thanks to the introduction on the market of the three axis autosampler. In light of the above, this contribution describes a novel user-friendly solid-phase microextraction (SPME) off- and on-line platform coupled with gas chromatography and triple quadrupole-mass spectrometry to determine urinary metabolites of polycyclic aromatic hydrocarbons 1- and 2-hydroxy-naphthalene, 9-hydroxy-phenanthrene, 1-hydroxy-pyrene, 3- and 9-hydroxy-benzoantracene, and 3-hydroxy-benzo[a]pyrene. In this new procedure, chromatography's sensitivity is combined with the user-friendliness of N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide on-fiber SPME derivatization using direct immersion sampling; moreover, specific isotope-labelled internal standards provide quantitative accuracy. The detection limits for the seven OH-PAHs ranged from 0.25 to 4.52 ng/L. Intra-(from 2.5 to 3.0%) and inter-session (from 2.4 to 3.9%) repeatability was also evaluated. This method serves to identify suitable risk-control strategies for occupational hygiene conservation programs.

Keywords: MTBSTFA; OH-PAHs; SPME; gas-chromatography.

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Conflict of interest statement

The authors declare no conflict of interest.

Figures

Figure 1
Figure 1
Derivatization of hydroxylated polycyclic aromatic hydrocarbons (OH-PAHs) with N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide (MTBSTFA).
Figure 2
Figure 2
Comparison between solid-phase microextraction fast fit fiber assemblies (SPME-FFA) Multi Off-Line Sampler (A) and SPME on-line (B) for the analysis of 60 urinary OH-PAHs samples.
Figure 3
Figure 3
The SPME Multi Off-Line Sampler.
Figure 4
Figure 4
Chromatogram of OH-PAHs by gas chromatography (GC)/triple quadrupole-mass spectrometry (QpQ-MS) in spiked artificial urine. A = 1-OH-Nap (200 ng/L); B = 2-OH-Nap (600 ng/L); C = 9-OH-Phen (50 ng/L); D = 1-OH-P (400 ng/L); E = 3-OH-B[a]A (1 ng/L); F = 9-OH-B[a]A (1 ng/L); G = 3-OH-B[p]A (5 ng/L).
See this image and copyright information in PMC

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