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三元醇丙烯酰胺键合色谱固定相的制备及评价
  • ISSN号:1000-8713
  • 期刊名称:色谱
  • 时间:2015.9
  • 页码:917-921
  • 分类:O658[理学—分析化学;理学—化学]
  • 作者机构:[1]生物医学分析化学教育部重点实验室,武汉大学化学系,湖北武汉430072
  • 相关基金:国家自然科学基金项目(21475098,91217309).
  • 相关项目:多种植物激素的同时检测方法学研究
中文摘要:

利用巯基与乙烯基的“点击化学”反应合成了一种新型含多羟基的硅烷偶联剂,再将其与硅胶反应制得含多羟基的亲水固定相。经过元素分析表征证明多羟基官能团已成功键合到硅胶表面。采用一系列不同性质的标准物质考察了亲水色谱模式下固定相的溶质保留机理。由于固定相结构中既具有极性多羟基官能团,也有短的疏水碳链,因此固定相兼具疏水性与亲水性。将此固定相成功应用于亲水与反相色谱两种模式,并对比了两种模式下流速对柱效的影响。最后将固定相应用于烷基苯、水溶性维生素以及核苷的分离中,取得了较好的分离效果,证明了固定相良好的应用前景。

英文摘要:

The present study described the preparation of N-acryloyltris( hydroxymethyl) amin-omethane-bonded silica ( NAS ) stationary phase based on “thiol-ene” click chemistry. The composition of the surface grafts of NAS stationary phase was determined by elemental analysis and the results demonstrated the successful introduction of the N-acryloyltris ( hydroxymethyl) aminomethane groups to the silica surface. Similar elemental composition of three batches of the NAS stationary phases exhibited good reproducibility of the preparation strategy. A set of standard compounds were employed to investigate the retention mechanism of the NAS station-ary phase by three different empirical equations. The results indicated the retention of the tested analytes on the NAS stationary phase was based more on a mixed-mechanism rather than a sim-ple partitioning or adsorption process. Eight compounds were selected to study the hydrophobic and hydrophilic properties of the NAS stationary phase in mobile phase with different ACN con-tents. Due to its hydrophilic triolacrylamide groups and short hydrophobic alkyl chains, the NAS phase was successfully applied in both reversed-phase liquid chromatography ( RPLC ) mode and hydrophilic interaction liquid chromatography ( HILIC) mode. The influence of flow rate on the column efficiency was compared in these two modes. In contrast to RPLC columns, the overall heights equivalent to a theoretical plate ( HETP ) in HILIC is weakly dependent on the retention of the analyte and the HETP curve is much flatter in RPLC than in HILIC at larger reduced velocities. Furthermore, the separation of alkylbenzenes, nucleosides and nucleobas-es, water-soluble vitamins was achieved on the new stationary phase, demonstrating the excel-lent application potential.

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期刊信息
  • 《色谱》
  • 北大核心期刊(2011版)
  • 主管单位:中国科学技术协会
  • 主办单位:中国化学会 中国科学院大连化学物理研究所
  • 主编:张玉奎
  • 地址:大连市中山路457号
  • 邮编:116023
  • 邮箱:sepu@dicp.ac.cn
  • 电话:0411-84379021
  • 国际标准刊号:ISSN:1000-8713
  • 国内统一刊号:ISSN:21-1185/O6
  • 邮发代号:8-43
  • 获奖情况:
  • 1998年获中国科学院科学出版基金择优支持(1998-2...,2001年获第四届中国科学院优秀期刊二等奖,2002年获第三届中国科协优秀期刊三等奖,连续多年被评为辽宁省一级期刊
  • 国内外数据库收录:
  • 俄罗斯文摘杂志,美国化学文摘(网络版),波兰哥白尼索引,荷兰文摘与引文数据库,美国生物医学检索系统,美国剑桥科学文摘,日本日本科学技术振兴机构数据库,中国中国科技核心期刊,中国北大核心期刊(2004版),中国北大核心期刊(2008版),中国北大核心期刊(2011版),中国北大核心期刊(2014版),英国英国皇家化学学会文摘,中国北大核心期刊(2000版)
  • 被引量:26730