Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.
J Chromatogr A. 2011 Dec 30;1218(52):9314-20. doi: 10.1016/j.chroma.2011.10.076. Epub 2011 Nov 15.
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%.
本文制备了两种苯并噻嗪键合硅胶（PTZ-Si）吸附剂，并将其用作固相萃取（SPE）的吸附剂，通过气相色谱-质谱联用（GC-MS）法测定环境水样中的硝基苯化合物。提出了不同的合成路线，以在硅胶表面获得高键合量的 PTZ。PTZ 分子被衍生为其氨基或酰氯衍生物，与异氰酸酯或氨基硅烷偶联剂反应，然后与硅胶表面的硅醇基团进一步反应，得到 PTZ-Si 吸附剂。通过氮气吸附孔隙率（NSP）、傅里叶变换红外光谱（FT-IR）和元素分析（EA）对所得的 PTZ-Si 吸附剂进行了表征，以确保 PTZ 成功键合到硅胶表面。然后，PTZ-Si 吸附剂被用作 SPE 吸附剂，用于富集硝基苯化合物。考察了影响萃取性能的几个参数。在优化条件下，该方法应用于环境水样中六种硝基苯化合物的分析。所有硝基苯化合物均具有良好的线性关系，R(2)均大于 0.9958。检测限范围为 0.06-0.3 ng/mL。在水样中添加的硝基苯化合物的方法回收率为 71.4%-124.3%，相对标准偏差（RSD）小于 10.1%。
