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A novel method for the determination of polycyclic aromatic hydrocarbons (PAHs) in water using Vacuum-assisted SPME Arrow

Anagnostou Eleni

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Summary

In this thesis, analyses were carried out on aqueous samples in order to detect polycyclic aromatic hydrocarbons, which are considered widespread environmental pollutants. The determination of these organic compounds was carried out using instrumental analysis and more specifically by applying Gas Chromatography coupled to Mass Spectrometry (GC MS). The isolation of the target compounds was achieved by applying the Arrow-type Solid Phase Microextraction technique under vacuum conditions, also known as Vacuum Assisted Headspace Solid Phase Microextraction Arrow (Vac-HS-SPME Arrow). The above method was optimized by studying the influence of the factors of extraction temperature and extraction time on the extraction efficiency of the target compounds. The results obtained under vacuum conditions were compared with those obtained under atmospheric pressure conditions (HS-SPME Arrow). In more detail, the use of Vac SPME Arrow resulted in faster extraction rates by applying mild heating for a shorter sampling time compared to HS-SPME Arrow. Furthermore, the application of vacuum significantly favored the extraction of less semi-volatile PAHs, while finally significant achievements were obtained regarding the extraction of PAH compounds of high volatility. The optimum extraction conditions for Nap, Phe, Flu compounds were found to be 15min of extraction while applying a mild temperature of 40oC for Vac SPME Arrow, while HS-SPME Arrow required heating at 60oC for the same sampling time. Therefore, the optimized Vac SPME Arrow method performed 1.5, 2 and 2.5 times higher sensitivity in the extraction of Nap , Phe and Flu respectively, but also wider linearity, lower detection limits, better repeatability than HS-SPME Arrow. Finally, the effect of the substrate (Matrix Effect) on the performance of the method was evaluated by performing PAH recovery experiments on real aqueous samples, revealing minimal effect of the matrix on extractions. All the above confirms the characterization of the Vac-HS-SPME Arrow technique as an easily applicable, sustainable, and economical practice, considering the robustness of Arrow combined with the large number of analyses, which can be used in both environmental and biological analyses and food analyses achieving excellent performance.

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