C18键合硅胶微球的制备及色谱分离性能  

Preparation and chromatographic separation of C18 bonded silica gel microspheres

作　　者：李鹏飞 王睿[1] 李冬云[1,2] 孙高梅琳 徐扬 葛洪良[1,2] LI Pengfei;WANG Rui;LI Dongyun;SUN Gaomeilin;XU Yang;GE Hongliang(College of Materials and Chemistry,China Jiliang University,Hangzhou 310018,China;National Center for Quality Testing of Magnetic Materials and Porducos,Hangzhou 310018,China;China National Inspection and Testing Holding Group Zibo Co.,Ltd.,Zibo 255035,China)

机构地区：[1]中国计量大学材料与化学学院,浙江杭州310018 [2]国家磁性材料质量监督检验检测中心,浙江杭州310018 [3]中国建材检验认证集团淄博有限公司,山东淄博255035

出　　处：《中国计量大学学报》2024年第3期480-486,共7页Journal of China University of Metrology

基　　金：浙江省领雁研发攻关计划项目(No.2023C03105)。

摘　　要：目的:制备出中位径为12μm的C18-SiO_(2)微球,并应用在色谱柱填料中,研究了影响微球形貌的制备因素及影响其液相分离的条件,获得制备C18-SiO_(2)微球的制备条件及影响其液相分离的条件。方法:以正硅酸乙酯(TEOS)为硅源,盐酸(HCl)为催化剂,十二烷基苯磺酸钠(C_(18)H_(29)NaO_(3)S)为表面活性剂,利用聚合诱导胶体凝聚法(PICA)合成介孔SiO_(2)微球,研究制备工艺(反应温度、pH值及甲醛和尿素的摩尔比N)对SiO_(2)微球大小形貌的影响规律,优化制备条件,制备出中位径为12μm SiO_(2)微球,经十八烷基三甲氧基硅烷(C_(21)H_(46)O_(3)Si)修饰后制备出C18-SiO_(2)微球,并用应用于高效液相色谱(HPLC)柱的填料,研究其对复合氨基酸的分离条件。结果:获得了中位径为12μm的C18-SiO_(2)微球的制备条件及液相分离条件。结论:利用PICA法成功制备了中位径为12μm的C18-SiO_(2)微球,粒径分布窄(D_(90)/D_(10)=1.63),介孔直径为10 nm,比表面积为236.38 m^(2)/g;在适宜的流动相和洗脱强度条件下,C18-SiO_(2)微球能够对复合氨基酸谷丙甘氨酸进行较快地分离,分离度均大于1.5。Aims:C18-SiO_(2) microspheres with a median diameter of 12μm were prepared and used in the column packing.The factors affecting the size and morphology of the microspheres and the conditions affecting the liquid phase separation were studied.The preparation conditions of C18-SiO_(2) microspheres and the conditions affecting the liquid phase separation were obtained.Methods:Using ethyl orthosilicate(TEOS)as the silicon source,hydrochloric acid(HCl)as the catalyst,and sodium dodecylbenzene the sulfonate(C_(18)H_(29)NaO_(3)S)as the surfactant,mesoporous SiO_(2) microspheres were synthesized by the polymerization-induced colloid condensation(PICA)method.The effect of preparation technology(reaction temperature,pH value and molar ratio N of formaldehyde and urea)on the size and morphology of SiO_(2) microspheres was studied;and the preparation conditions were optimized to prepare SiO_(2) microspheres with a median diameter of 12μm.C18-SiO_(2) microspheres were prepared after modification by octadecyl trimethoxysilane(C_(21)H_(46)O_(3)Si).The separation conditions of complex amino acids were studied by using it as the filler for high performance liquid chromatography(HPLC)columns.Results:The preparation conditions and liquid phase separation conditions of C18-SiO_(2) microspheres with a median diameter of 12μm were obtained.Conclusions:C18-SiO_(2) microspheres with a median diameter of 12μm were successfully prepared by the PICA method,with a narrow particle size distribution(D_(90)/D_(10)=1.63),a mesoporous diameter of 10 nm,and a specific surface area of 236.38 m^(2)/g.Under suitable conditions of mobile phase and elution strength,C18-SiO_(2) microspheres can quickly separate the complex amino acid glutamic acid;and the separation degree is over 1.5.

关 键 词：介孔SiO_(2)微球 液相色谱填料 谷丙甘氨酸 C18-SiO_(2)微球 

分 类 号：TB195.6[一般工业技术]