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

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.

Durable molybdenum oxide coated solid‐phase microextraction fiber for highly selective and efficient extraction of polycyclic aromatic hydrocarbons in water

“…Solid‐phase microextraction is a fast, sensitive, simple, and solvent‐free technique and has attracted immense attention since it was introduced by the Arthur and Pawliszyn research groups in 1990 . An important part of the SPME technique is the SPME fiber, which consists of a substrate and a coating to adsorb analytes from the samples.…”

Recent applications of microextraction sample preparation techniques in biological samples analysis

“…One year later Dugheri et al (2018) developed a novel userfriendly SPME off-and online platform coupled with GC and triple quadrupole-MS for analysis of seven OH-polycyclic aromatic hydrocarbons (PAHs) including 1-and 2-hydroxy-naphthalene, 9-hydroxyphenanthrene, 1-hydroxy-pyrene, 3-and 9-hydroxy-benzoantracene and 3-hydroxy-benzo [a]pyrene in urine samples (Dugheri et al, 2018).…”

Solid phase microextraction techniques used for gas chromatography: a review

“…SPME, Twister W , and MonoTrap TM have proven to be among the most performing and versatile devices for environmental sampling, in particular for air sampling [65][66][67][68][69]. To face the needed of high-throughput analytical sessions, special systems for these microextraction techniques, Multi Fiber eXchange (MFX, EST, Fairfield, USA) for SPME fibers and Thermal Desorption Unit tray (Gerstel, Mülheim an der Ruhr, Germany) for Twister W and MonoTrap TM , were developed; they allow not only on-line sampling and injecting but also the upload of multiple samplers, which once sampled off-line and can then processed in complete automation, thanks to the dedicated autosampler systems [70].…”