Headspace single drop microextraction combined with HPLC for the determination of trace polycyclic aromatic hydrocarbons in environmental samples

This study describes an analytical method employing capillary gas chromatography (GC) using flame ionization detection (FID) that has been developed for the simultaneous determination of polycyclic aromatic hydrocarbons (PAHs) in wastewater, including naphthalene, 1-naphthol, 2-naphthol and anthracene. For this purpose, single-drop microextraction (SDME) was applied as a sample preparation technique. The SDME parameters such as types of extractants, volume of the microdroplet size, extraction time, stir rate and immersion depth of needle point were investigated and optimized. The method was linear in the ranges from 2.3 ×10-3to 70.0 μg·mL-1for naphthalene, 1-naphthol and anthracene, and 2.2 ×10-3to 50.0 μg·mL-1for 2-naphthol withR2≥ 0.9990. The SDME procedure allowed efficient recovery of the investigated PAHs ranging between 94 % and 104 % with a relative standard deviation (RSD) ≤4.2 for actual wastewater sampes spiked with 5, 10 and 20 μg·mL-1of PAHs, respectively. These results showed the potential of this technique for PAHs monitoring in wastewater samples. Furthermore, the investigated methods are simple, reliable, reproducible, and not expensive.

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Evaluation of a Simplified Method for GC/MS Qualitative Analysis of Polycyclic Aromatic Hydrocarbons, Polychlorinated Biphenyls, and Organic Pesticides Using PARADISe Computer Program

Molecules ◽

10.3390/molecules25163727 ◽

2020 ◽

Vol 25 (16) ◽

pp. 3727

Author(s):

Łukasz Dąbrowski

Keyword(s):

Polycyclic Aromatic Hydrocarbons ◽

Polychlorinated Biphenyls ◽

Computer Program ◽

Aromatic Hydrocarbons ◽

Environmental Samples ◽

Organic Carbon Content ◽

Standard Mixture ◽

Polycyclic Aromatic ◽

Organic Pesticides

For complex matrices such as environmental samples, there is usually a problem with not fully resolved peaks during GC/MS analysis. The PARADISe computer program (based on the PARFAC2 model) allows the identification of peaks using the deconvoluted mass spectra and the NIST MS library. The number of repetitions required by this software (at least five) is a real limitation for the determination of semi-volatile compounds, like polycyclic aromatic hydrocarbons, polychlorinated biphenyls, and organic pesticides in environmental samples. In this work, the method to overcome this condition was proposed and evaluated. The sets of the five files required by PARADISe were prepared by mathematically modifying the original GC/MS chromatograms obtained for the standard mixture (C = 2 µg/mL of 40 compounds) and real sample extracts (soil samples with different total organic carbon content and one cardboard extract) spiked with standards. Total average match factor for all the substances identified in a standard mixture was 874 (near 900—“excellent match”), and for all the substances in the real samples, it was 786 (near 800—“good match”). The results from PARADISe were comparable to those obtained with other programs: AMDIS (NIST) and MassHunter (Agilent), tested also in this work. PARADISe software can be effectively used for chromatogram deconvolution and substance identification.

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