Assessing method performance for polycyclic aromatic hydrocarbons analysis in sediment using GC-MS: method validation and principal component analysis for quality control

Abstract

ABSTRACT Polycyclic aromatic hydrocarbons (PAHs) belong to the persistent organic pollutant class and are ubiquitously present in the environment. As a consequence of their high hydrophobicity, PAHs in aquatic environments tend to rapidly sink down to the bottom sediments which are the most important reservoirs of PAHs in the aquatic environment. This paper presents the validation and further performance evaluation of a method modified in-house for PAHs’ sample preparation and analysis in sediment using gas chromatography-mass spectrometry (GC-MS). The method validation covers determining the calibration linear range, method detection and quantitation limits, method recovery and precision, method uncertainty and further internal and external quality control steps. Principal component analysis was used to identify the influence of different variables on method performance and indicated main clustering by PAH molecule size. The results of a two-year quality control programme show that the variations in method performance were not statistically significant in comparison to the parameters set during the validation experiments. Trueness expressed as recovery was very similar for spiked sediment samples and the analysed certified reference material (CRM) (70.6–113%). Expanded uncertainty ranged from 40.4% to 50.9% with higher values noted for the highly hydrophobic PAHs benzo(a)pyrene and benzo(g,h,i)perylene.