School of Pharmaceutical Science & Technology, Tianjin University, 92 Weijin Road, Tianjin, 300072, China.
School of Pharmaceutical Science & Technology, Tianjin University, 92 Weijin Road, Tianjin, 300072, China.
J Chromatogr A. 2020 May 10;1618:460866. doi: 10.1016/j.chroma.2020.460866. Epub 2020 Jan 13.
An energy-efficient and environment-friendly approach to prepare porous monodispersed micro-sized silica particles with methyltrimethoxysilane (MTMS) as the precursor is described. The particles were synthesized by a two-step hydrolysis/condensation procedure, with post-synthetic aging and calcination for methyl group removal. They show uniform spherical morphology, narrow particle size distribution (D/, 1.2-1.6), tailored particle size (3, 5, 7 μm) and mesopore structure (10, 13 nm), which can be directly used as packing materials for HPLC without size classification. C, sulfonate, and C/sulfonate mixed-mode stationary phases were produced by a green vapor deposition method based on the synthesized silica particles. The newly synthesized C phase exhibits mechanical stability, kinetic behavior and separation performance expected from the commercial C column. The C/sulfonate phase exhibits prominent mixed-mode retention behavior which can be applied to the simultaneous separation of multiple substances in the compound drugs.
一种以甲基三甲氧基硅烷（MTMS）为前驱体，制备具有高效节能和环保特性的多孔单分散微尺度二氧化硅颗粒的方法。该颗粒采用两步水解/缩合法合成，经后合成老化和煅烧除去甲基。这些颗粒具有均匀的球形形貌、窄的粒径分布（D/，1.2-1.6）、可调节的粒径（3、5、7μm）和介孔结构（10、13nm），无需进行粒径分级即可直接用作 HPLC 的填充材料。基于合成的二氧化硅颗粒，采用绿色气相沉积法制备了磺酸酯和 C/磺酸酯混合模式固定相。新合成的 C 相表现出与商业 C 柱相当的机械稳定性、动力学行为和分离性能。C/磺酸酯相表现出显著的混合模式保留行为，可用于同时分离复方药物中的多种物质。
