Zhao Zhenzhen, Qu Qishu, Zhang Xinxin, Gu Xue, Wang Yan, Yan Chao
School of Pharmacy, Shanghai Jiao Tong University, Shanghai, China.
Se Pu. 2009 Jul;27(4):431-5.
Gold microspheres modified with octadecanethiol as chromatographic stationary phase were prepared. The particles were characterized by the scanning electron micrograph (SEM), Fourier transform infrared spectroscopy (FT-IR), elemental analysis and nitrogen adsorption analysis. The average diameter, the surface area and the average pore diameter were 3.5 microm, 49.0 m2/g and 5.0 nm, respectively. The IR spectra demonstrated that C18 was bonded to the surface of gold microspheres with the carbon content of 0.56%. Using these microspheres as stationary phase, a 19 cm section of a total length of 36 cm capillary (100 microm i. d.) was packed electrokinetically, and the evaluations in capillary liquid chromatography and pressurized capillary electrochromatography were performed. The mobile phases (80% methanol) with extreme pH values (pH 1.0 or pH 12.0) were used to flush the column for 140 h. In order to investigate the chemical stability of the column, the retention factors before and after flushing were calculated and compared based on the experimental results. There was no remarkable deterioration on the retention factors after flushing, which demonstrated the column was stable pounds were separated using capillary liquid chromatography to examine the retention behavior of the column, and over 50,000 theoretical plates per meter and acceptable symmetry peaks were obtained. The pressurized capillary electrochromatographic properties of the column were investigated using a separation of the mixture of aniline and benzoic acid, and the separation was obtained when a 5 kV positive or negative voltage was applied. The research work confirmed the feasibility of using the octadecanethiol modified gold microspheres as a novel stationary phase for capillary liquid chromatography and pressurized capillary electrochromatography.
制备了用十八烷硫醇修饰的金微球作为色谱固定相。通过扫描电子显微镜（SEM）、傅里叶变换红外光谱（FT-IR）、元素分析和氮吸附分析对颗粒进行了表征。平均直径、表面积和平均孔径分别为3.5微米、49.0平方米/克和5.0纳米。红外光谱表明C18以0.56%的碳含量键合到金微球表面。使用这些微球作为固定相，对一根全长36厘米（内径100微米）毛细管中的19厘米部分进行电动填充，并进行了毛细管液相色谱和加压毛细管电色谱评估。使用极端pH值（pH 1.0或pH 12.0）的流动相（80%甲醇）冲洗柱子140小时。为了研究柱子的化学稳定性，根据实验结果计算并比较了冲洗前后的保留因子。冲洗后保留因子没有明显恶化，这表明柱子是稳定的。使用毛细管液相色谱分离化合物以检查柱子的保留行为，每米获得了超过50,000个理论塔板和可接受的对称峰。使用苯胺和苯甲酸混合物的分离研究了柱子的加压毛细管电色谱性能，当施加5 kV正电压或负电压时实现了分离。该研究工作证实了使用十八烷硫醇修饰的金微球作为毛细管液相色谱和加压毛细管电色谱新型固定相的可行性。
