Preparation of phenothiazine bonded silica gel as sorbents of solid phase extraction and their application for determination of nitrobenzene compounds in environmental water by gas chromatography–mass spectrometry

In this paper, two phenothiazine bonded silica (PTZ-Si) sorbents were prepared and used as sorbents of solid-phase extraction (SPE) for the determination of nitrobenzene compounds in environmental water samples by gas chromatography–mass spectrometry (GC–MS). Different synthesis routes were proposed to obtain high bonded amount of PTZ on the surface of silica gel. PTZ molecule was derived to its amino or acyl chloride derivatives for reacting with isocyanate or amino silane coupling agent, which was further reacted with the surface silanol groups of silica gel to obtain the PTZ-Si sorbents. The resultant PTZ-Si sorbents were characterized by nitrogen sorption porosimetry (NSP), Fourier transform infrared spectroscopy (FT-IR) and elemental analysis (EA) to assure the successful bonding of PTZ on the surface of silica gel. Then the PTZ-Si sorbents were served as SPE sorbents for the enrichment of nitrobenzene compounds. Several parameters affecting the extraction performance were investigated. Under the optimized conditions, the proposed method was applied to the analysis of six nitrobenzene compounds in environmental water samples. Good linearities were obtained for all nitrobenzene compounds with R2 larger than 0.9958. The limits of detection were found to be in the range of 0.06–0.3 ng/mL. The method recoveries of nitrobenzene compounds spiked in water samples were from 71.4% to 124.3%, with relative standard deviations (RSDs) less than 10.1%.

► Two approaches were proposed to prepare phenothiazine bonded silica (PTZ-Si) gel.
► The PTZ-Si SPE sorbents were used for the enrichment of nitrobenzene compounds.
► Good performance for the extraction of nitrobenzene compounds was achieved.
► GC–MS was adopted for the separation and detection of nitrobenzene compounds.
► A determination method of nitrobenzene compounds in water samples was established.