摘要
采用２，４－戊二酮与正辛烷基二甲基氯硅烷反应制成活泼的中间体——硅醚型硅烷中间体，然后再与硅胶进行键合。经元素分析、漫反射红外光谱和高效液相色谱法对键合相进行了鉴定和评价。结果表明，键合反应按预定路线进行，硅胶表面被键合相基团覆盖的较均匀、完全。键合相具有较好的色谱性能，可有效地用于碱性化合物的分离分析中。
A bonded phase for high performance liquid chromatography(HPLC) has been prepared by the new reaction between silica and silicon ether. The ether was synthesized from alkylchlorosilane and pentane 2,4 dione in the presence of imidazole under inert conditions by using anhydrous tetrahydrofuran as solvent. The bonded phase thus obtained was characterized by elemental analysis, diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy and HPLC evaluation. The carbon content was 9.4% and the surface coverage almost attained 3.0μmol/m 2 without end capping. The silanol absorption peaks of the product cannot be observed from the DRIFT spectrum, which revealed that the silanization reaction proceeded thoroughly. The basic solutes, such as aniline, o toluidine, p toluidine, N,N dimethylaniline and pyridine were used as the probe solutes to examine their interaction with the residual silanols on the surface of the products. No buffer or salt was used in the mobile phase for these experiments. In comparison with an acidic solute, such as, phenol, basic aniline eluted in front of phenol, and the ratio of asymmetry of aniline peak to that of the phenol peak was 1.1. Furthermore the relative k′ value of p toluidine to that of o toluidine was also 1.1. All the results showed that the stationary phase has better quality and reproducibility and can be used for the separation of basic solutes efficiently.
出处
《色谱》
CAS
CSCD
北大核心
1997年第3期189-192,共4页
Chinese Journal of Chromatography
关键词
高效液相色谱法
键合固定相
碱性化合物分离
high performance liquid chromatography, stationary phase, separation of basic solutes
