title: 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.
abstract: 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 R(2) 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%.
authors: Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.
authors: Xi-Tian
authors: XT
authors: Peng
authors: Xing
authors: X
authors: Zhao
authors: Yu-Qi
authors: YQ
authors: Feng
mesh_terms: D004136:Dinitrobenzenes / Q000032:analysis* / Q000302:isolation & purification; D005618:Fresh Water / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D057230:Limit of Detection; D016014:Linear Models; D010640:Phenothiazines / Q000737:chemistry*; D015203:Reproducibility of Results; D058428:Silica Gel / Q000737:chemistry; D052616:Solid Phase Extraction / Q000379:methods*; D017550:Spectroscopy, Fourier Transform Infrared; D014050:Toluene / Q000031:analogs & derivatives* / Q000032:analysis / Q000302:isolation & purification; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification
chemical_list: D004136:Dinitrobenzenes; D010640:Phenothiazines; D014874:Water Pollutants, Chemical; D014050:Toluene; D058428:Silica Gel; C031637:phenothiazine