中文摘要：

针对在线固相萃取-液相色谱联机分析中的萃取柱及阀体系与液相色谱兼容的问题进行研究，构建了与液相色谱进样量相兼容的大内径整体萃取柱及相关阀、泵送系统。采用四甲氧基硅烷（TMOS）和甲基三甲氧基硅烷（MTMS）作为混合前驱体，制备了大内径（530μm）、柱床均一、稳定的毛细管硅胶整体柱。经C18基团修饰后，前沿分析表明该整体柱具有大的吸附容量，其中N-甲基苯胺约为214mg／g，N，M二甲基苯胺约为388mg／g。柱通透性好，在线固相萃取时仅需注射泵即可完成。将该整体柱应用于本实验室自主研发的样品前处理仪上并与液相色谱联机后，采用85％甲醇-水作为流动相，在0．5mL／min的流速和254nm紫外检测波长下对水中痕量苯胺类化合物进行在线富集与分离分析。在0．1，1和10mg／mL添加水平下，湘江水中苯胺类化合物的回收率为81．9％～91．3％；日内与日间相对标准偏差均低于7．6％。

英文摘要：

For extraction column and valve system compatibility issues in on-line SPE -liquid chromatography analysis, we have built the large inner diameter extraction monolithic column compatible with liquid chromatography and related valve, pumping system. A large inner diameter （530 μm i. d. ）, uniform and stable silica monolithic capillary column has been prepared by using two hybrid precursor -tetramethoxysilane and methyltrimethoxysilane. After the modification of C18 group, the results of frontier analysis show that the monolithic column has a larger adsorption capacity, wherein N-methylaniline is approximately 214 g/g, and N, N-Dimethylaniline is about 388 g/g. The column permeability is good, so the on-line solid phase extraction can be completed requires only the injection pump. The monolithic column was connected to the sample preparation equipment made by our laboratory and with the combination of liquid chromatography for online enrichment and separation, and it was applied to the determination of trace aniline categories compounds in river water. The mobile phase consisted of 15% methanol and 85% water solution in volume ratio; the flow rate for chromatographic separation was 0.5 mL/min; the detection wavelength was 254 nm. The recoveries were in the range of 81.9%-91.3%, and the relative standard deviation（RSDs） of intraday and interday were not larger than 7.6% at 0.1, 1 and 10 g/L three spiked levels for all analytes.