[Preparation and evaluation of octadecanethiol modified gold microspheres in capillary liquid chromatography and pressurized capillary electrochromatography as stationary phase].
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.
Zhao
Zhenzhen
Z
School of Pharmacy, Shanghai Jiao Tong University, Shanghai, China.
Qu
Qishu
Q
Zhang
Xinxin
X
Gu
Xue
X
Wang
Yan
Y
Yan
Chao
C
D002853:Chromatography, Liquid / Q000295:instrumentation* / Q000379:methods; D019075:Electrophoresis, Capillary / Q000295:instrumentation* / Q000379:methods; D006046:Gold / Q000737:chemistry*; D008863:Microspheres; D013438:Sulfhydryl Compounds / Q000737:chemistry*
D013438:Sulfhydryl Compounds; C055360:n-octadecyl mercaptan; D006046:Gold