Simple multi-residue analysis of persistent organic pollutants and molecular tracers in atmospheric samples

Minas Iakovides; Jean Sciare; Nikos Mihalopoulos

doi:10.1016/j.mex.2023.102224

Simple multi-residue analysis of persistent organic pollutants and molecular tracers in atmospheric samples

MethodsX. 2023 May 17:10:102224. doi: 10.1016/j.mex.2023.102224. eCollection 2023.

Authors

Minas Iakovides¹, Jean Sciare¹, Nikos Mihalopoulos^{1

2

3}

Affiliations

¹ Climate and Atmosphere Research Center (CARE-C), The Cyprus Institute, 20 Konstantinou Kavafi Str., Aglantzia 2121, Cyprus.
² Chemistry Department, University of Crete, Heraklion Crete 71003, Greece.
³ Institute for Environmental Research and Sustainable Development, National Observatory of Athens, Palaia Penteli, Athens 15236, Greece.

Abstract

We present a simple, selective and sensitive analytical method to quantitatively determine a wide range of halogenated persistent organic pollutants and molecular tracers in atmospheric samples. Identification and quantification was carried out by high-resolution gas chromatography, hyphenated with low-resolution mass spectrometry operating in electron impact (EI) and electron capture negative ionization (ECNI) mode. Optimization on a number of instrumental parameters was conducted to obtain ultra-trace detection limits, in the range of few fg/m³ for organohalogen compounds. Repeatability and reproducibility of the method was thoroughly evaluated. The analysis was validated with standard reference materials and successfully applied to actual atmospheric samples. The proposed multi-residue method provides a precise, affordable and practical procedure of sample analysis for environmental research laboratories with conventional instrumentation on a routine basis.•A simple combination of alumina, florisil and silica gel adsorbents was applied to sufficiently isolate polychlorinated biphenyls, organochlorine pesticides, polycyclic aromatic hydrocarbons, long chain n-alkanes, hopanes and steranes.•Full elution was achieved in two successive fractions, using small volumes of n-hexane and n-hexane/dichloromethane to recover all target substances.•To maximize analytical response, optimization was applied for three operating parameters in ECNI mode: i) ion source temperature; ii) emission current; and iii) electron energy.

Keywords: GC/MS; Hopanes; Negative chemical ionization; OCPs; Optimization; PAHs; PCBs; Simple multi-residue analysis of persistent organic pollutants and molecular tracers in atmospheric samples.; Steranes.