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.
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.
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DOI：
10.1016/j.chroma.2011.10.076
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发表时间：
2011-12
期刊：
影响因子：
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通讯作者：
Xitian Peng;Xingzhong Zhao;Yuqi Feng
中科院分区：
文献类型：
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作者：
Xitian Peng;Xingzhong Zhao;Yuqi Feng
制备了两种吩噻嗪键合硅胶（PTZ-Si）吸附剂，并将其作为固相萃取（SPE）吸附剂，应用气相色谱-质谱（GC-MS）法测定环境水样中的硝基苯类化合物。提出了不同的合成路线，以获得高键合量的硅胶表面的PTZ。将PTZ分子衍生为氨基或酰氯衍生物，与异氰酸酯或氨基硅烷偶联剂反应，再与硅胶表面的硅醇基团反应，得到PTZ-Si吸附剂。采用氮气吸附法（NSP）、傅立叶变换红外光谱（FT-IR）和元素分析（EA）对所制备的PTZ-Si吸附剂进行了表征。然后将PTZ-Si吸附剂作为固相萃取吸附剂用于硝基苯类化合物的富集。研究了影响萃取性能的几个参数。在优化的条件下，将该方法应用于环境水样中6种硝基苯类化合物的分析。硝基苯类化合物的线性关系良好，R2> 0.9958。方法的检出限为0.06-0.3ng/mL。水样中硝基苯类化合物的加标回收率为71.4%~ 124.3%，相对标准偏差小于10.1%。
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 R2larger than 0.9958. The limits of detection were found to be in the range of 0.06–0.3ng/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%.