Headspace solid-phase-microextraction using a graphene aerogel for gas chromatography-tandem mass spectrometry...

Polychlorinated naphthalenes (PCNs) are emerging organic pollutants that are harmful to the environment and human health. In this study, a headspace solid-phase-microextraction (HS-SPME)-gas chromatography-tandem mass spectrometry method for the separation and enrichment of PCNs in shrimp was developed and validated. A graphene aerogel was prepared by modifying graphene oxide with a deep eutectic solvent to prevent graphene oxide stacking. As a result, the aerogel had a three-dimensional porous structure, which resulted in easy sorption/desorption for PCNs, and was used as the SPME fiber coating. Next, the experimental parameters for the saponification of the sample matrix and the extraction and desorption of the PCNs were systematically optimized. After optimization, the method showed good linearity (R²≥0.9968), low limits of detection (0.00983-0.0661 pg g^-1), and satisfactory recoveries (80.4-108%). Crucially, compared with previously reported methods, this method does not require the use of large amounts of organic reagents or complex operations, giving it the advantages of simplicity, sensitivity, and environmental friendliness. As an example of the practical application of the developed method, the PCNs in river and sea shrimp were quantified.