Yang Zhao, Jie Li, Yang Yang, Yujie Bi, Changyu Cai, Yanxiong Ke
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引用次数: 0
摘要
本研究在常压下通过假形态转化法合成了孔径在 30 到 200 Å 之间的球形二氧化硅。通过使用季胺阳离子表面活性剂和不同种类的膨胀剂(包括聚丙二醇、1,3,5-三甲基苯、烷烃和烷醇),获得了孔径分布较窄的 40-80 埃二氧化硅颗粒。所有这些二氧化硅颗粒都可以在温和的条件下于 12 小时内合成,为制备孔径可调的色谱基质提供了一种简便的合成方法。该方法重现性好,按比例放大制备的二氧化硅球孔隙结构参数的相对标准偏差小于 6%。在尺寸排阻色谱法中研究了孔径对低分子量肝素(LMWH)组分的影响。不同孔径分布的基质具有不同的尺寸排除区域。通过在双柱循环分离过程中使用 UPS-60-Diol 色谱柱,在 5 个柱体积内分离出分子量在 3000-8000 Da 范围内的 LMWH,其中肝素含量为 85%。
Pseudomorphic synthesis of pore size-tunable mesoporous silica spherical particles and their application for the fraction of low-molecular-weight heparin
In this study, spherical silica with pore size varied from 30 to 200 Å was synthesized by pseudomorphic transformation at atmospheric pressure. 40–80 Å silica particles with a narrow pore distribution were obtained by using quaternary amine cationic surfactants and different kinds of swelling agents, including polypropylene glycol, 1,3,5-trimethylbenzene, alkanes, and alkanols. Alkyl imidazolium ionic liquid surfactants were used to synthesize large pore size distribution silica spheres with pore sizes in the range of 110–200 Å. All these silica particles can be synthesized under mild conditions within 12 h, which provides a facile synthesis method for the preparation of a chromatographic matrix with tunable pore size. The method is reproducible and the relative standard deviation of silica sphere pore structure parameters in scaled-up preparations is less than 6%. The pore size on the fraction of low-molecular-weight heparin (LMWH) was investigated in size exclusion chromatography. Matrixes with different pore size distributions have various size exclusion regions. By using UPS-60-Diol columns in a twin-column recirculation separation process, LMWH with >85% heparin with molecular weight within the range of 3000–8000 Da were separated in five-column volumes.
期刊介绍:
The Journal of Separation Science (JSS) is the most comprehensive source in separation science, since it covers all areas of chromatographic and electrophoretic separation methods in theory and practice, both in the analytical and in the preparative mode, solid phase extraction, sample preparation, and related techniques. Manuscripts on methodological or instrumental developments, including detection aspects, in particular mass spectrometry, as well as on innovative applications will also be published. Manuscripts on hyphenation, automation, and miniaturization are particularly welcome. Pre- and post-separation facets of a total analysis may be covered as well as the underlying logic of the development or application of a method.