烷基化聚甲基倍半硅氧烷色谱填料的制备与其反相保留机理探究  

PREPARATION OF ALKYLATED POLYMETHYLSESQUISILOXANE CHROMATOGRAPHIC PACKING AND STUDY OF ITS REVERSE PHASE RETENTION MECHANISM

作　　者：李佳丽 LI Jiali(School of Pharmaceutical Science and Technology, Tianjin University Tianjin 300072, Chin)

机构地区：[1]天津大学药物科学与技术学院,天津300072

出　　处：《离子交换与吸附》2018年第2期168-177,共10页Ion Exchange and Adsorption

摘　　要：以甲基三甲氧基硅烷(MTMS)和巯丙基三甲氧基硅烷(MpTMS)为原料利用二步酸碱催化水解缩聚法,制备得到了多孔单分散性巯丙基功能化聚甲基倍半硅氧烷微球(Mp-PMSQ)。然后通过"巯基-乙烯基"点击化学反应,成功将微球烷基化,制备得到了具有不同C_(12)浓度的烷基化(C_(12)-S-PMSQ)微球。结果表明,该类微球单分散性良好、粒径分布较窄(D90/D10<1.5);烷基化后随着C_(12)浓度的增加,对应微球的孔结构参数减小而碳含量增加。采用苯同系物对其进行反相色谱行为评价,发现随着C_(12)浓度的增加,苯同系物的保留因子下降,因此我们推测吸附机理为其主导反相保留机理。The methyltrimethoxylsilane （MTMS） and mercaptopropyltrimethoxysilane （MpTMS） were used as precursors to prepare monodispersed porous mercaptopropyl-functionalized polymethylsilsesquioxane （Mp-PMSQ） particles. Then, a series of C12-S-PMSQ particles with different ligand density （Dodecene） were successfully prepared through the alkylation of Mp-PMSQ by ＂thiol-ene＂ click chemistry. The results showed that the particles have good monodispersity and narrow particle size distribution （D90/D10〈1.5）; After alkylation with the increasing of alkyl chain length, the pore structure parameters decreased but the carbon content of obtained particles increased. The reversed phase chromatographic evalution were carried out by using benzene homologues as analytes. It was found that the retention factor of benzene homologues were decreased with the increasing of alkyl chain density of obtained particles.

关 键 词：反相色谱填料 聚倍半硅氧烷 “巯基-乙烯基”点击化学 碳链浓度 吸附机理 

分 类 号：O631.5[理学—高分子化学]