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期刊信息
  • 主管单位:
  • 上海市教育委员会
  • 主办单位:
  • 上海理工大学
  • 主  编:
  • 庄松林
  • 地  址:
  • 上海市军工路516号
  • 邮政编码:
  • 200093
  • 联系电话:
  • 021-55277251
  • 电子邮件:
  • xbzrb@usst.edu.cn
  • 国际标准刊号:
  • 1007-6735
  • 国内统一刊号:
  • 31-1739/T
  • 邮发代号:
  • 4-401
  • 单  价:
  • 15.00
  • 定  价:
  • 90.00
张璐,王照地,刘璐,王世革,黄明贤.硅胶整体柱的研磨与表面修饰制备新型高效液相色谱固定相[J].上海理工大学学报,2020,42(2):122-130.
硅胶整体柱的研磨与表面修饰制备新型高效液相色谱固定相
Preparation of new stationary phases in high performance liquid chromatography with the surface modification on a ground silica monolith colume
投稿时间:2019-03-07  
DOI:10.13255/j.cnki.jusst.20190307001
中文关键词:  硅胶整体柱  巯基-烯点击反应  限进介质色谱固定相
英文关键词:silica monolith column  thiol-ene click reaction  restricted access media stationary phase
基金项目:上海市科委项目(14440502300);上海理工大学沪江基金资助项目(D15011)
作者单位E-mail
张璐 上海理工大学 理学院, 上海 200093  
王照地 上海理工大学 理学院, 上海 200093  
刘璐 上海理工大学 理学院, 上海 200093  
王世革 上海理工大学 理学院, 上海 200093  
黄明贤 上海理工大学 理学院, 上海 200093 hmx@usst.edu.cn 
摘要点击次数: 100
全文下载次数: 91
中文摘要:
      研究以聚乙二醇(PEG)为致孔剂,以四甲氧基硅烷(TMOS)为硅源,在醋酸和尿素的催化作用下水解缩合成硅胶整体柱;将此整体柱研磨、煅烧和浮选,制备了不定型介孔硅胶颗粒。控制反应时间为48 h、反应温度为先40 ℃再120 ℃、研磨速度为150 r/min、研磨时间为1 h,可得到孔径为16 nm左右、粒径范围在4~6 μm的支架型硅胶颗粒。在此基础之上,通过不同的表面修饰方法,制备了表面键合的含双键C8反相色谱固定相,通过巯基−烯点击反应和表面聚合反应进一步制备了2种新型反相色谱固定相,以及通过巯基−环氧反应制备了限进介质色谱固定相。进行了针对塑化剂和牛血清中药物的色谱分离测试,结果显示,基于上述方法得到的高效液相色谱填料具有一定的实际应用潜力。
英文摘要:
      A silica monolith column was prepared with polyethylene glycol (PEG) as a porogen, tetramethoxysilane (TMOS) as a silica precursor, as well as acetic acid and thermally decomposed urea as catalysts. The silica monolith column was then ground by a ball-mill, calcined and selected by floatation to obtain 4~6 μm silica particles. For the preparation of monolithic silica, the process was: first, 48 h reaction at 40 ℃ reaction temperature, and then another 48 h reaction at 120 ℃ reaction temperature. For the preparation of silica particles, the grinding speed was 150 r/min, and the grinding time was 1 h. The silica particles with the pore size of about 16 nm and the particle size ranged in 4~6 μm were obtained. With different modification methods on the surface of the as-prepared silica particles, a series of new stationary phases were prepared, including the surface bonded vinyl group containing C8 reverse phase, thiol-ene click reaction and free radical polymerization produced new reverse phases, and thiol-epoxy reaction generated restricted access media stationary phase. The chromatographic separation for plasticizers and drugs in bovine serum albumin (BSA) was conducted, and the results show that the packing materials so prepared have potentials for practical applications in high performance liquid chromatography (HPLC).
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