Preparation and evaluation of amino modified graphene solid-phase microextraction fiber and its application to the determination of synthetic musks in water samples

In the current study, amino modified (NH2-modified) graphene was developed as a solid-phase microextraction (SPME) coating for the first time. The structure of the NH2-modified graphene was characterized by X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). The fiber was fabricated using xylene-diluted silicone sealant as an adhesion agent. The performance and feasibility of the NH2-modified graphene fiber was evaluated through autosampler-assisted direct immersion (DI) SPME followed by gas chromatography-mass spectrometry (GC/MS) for the analysis of five synthetic musks (muscone, galaxolide, musk-xylene, tonalide and musk-ketone) in aqueous samples. The results showed that the prepared fiber had good thermal stability, excellent solvent resistance and a long service lifetime (more than 200 replicate extraction cycles). The proposed autosampler-assisted DI-SPME-GC/MS method showed low limits of detection (0.46-5.96 ng L−1), wide linear ranges (5-500 ng L−1), and acceptable reproducibility (relative standard deviation, RSD < 12%). Finally, the method was successfully applied to the analysis of synthetic musks in environmental water samples with good recoveries (82.3-112%) and satisfactory precisions (RSD < 9.9%). These results indicated that the NH2-modified graphene provided a promising alternative in sample pretreatment.