后交联法制备大孔吸附树脂及其对灯盏乙素的分离研究  

PREPARATION OF MACROPOROUS RESIN BY POST-CROSSLINKING METHOD FOR SEPARATION OF SCUTELLARIN

作　　者：李世东[1] 徐环昕[1,2] 刘坐镇[1,2] 宁方红[1,2] 江邦和[1,2] 

机构地区：[1]华东理工大学生物反应器工程国家重点实验室,上海200237 [2]上海华震科技有限公司,上海200237

出　　处：《离子交换与吸附》2014年第4期376-384,共9页Ion Exchange and Adsorption

摘　　要：通过种球溶胀法合成的粒径为15μm,交联度为80%的聚(苯乙烯-二乙烯苯)微球(PS-DVB),以三氯化铁为催化剂,通过悬挂双键后交联反应,制备出具有较高比表面积的大孔吸附树脂色谱填料;利用上述色谱填料装填成规格为4.6mm×250mm的色谱柱,对灯盏乙素进行高效液相色谱分离,以分离度、选择因子、柱效和保留时间为考察指标,研究了流动相比例、流动相流速、柱温和进样浓度等对分离过程的影响。在流动相为乙腈:0.4%冰乙酸(27:73,v:v),流速为1.0mL/min,柱温为30℃,进样浓度为300μg/mL的条件下,灯盏乙素和灯盏甲素的分离度为2.20,两组分可完全分离,保留时间为7.1min,为灯盏乙素的大规模制备提供了可能。Macroporous resin with high specific surface area was prepared by post-crosslinkingreaction of polystyrene microspheres with particle size of 15μm and degree of crosslinking of80% using ferric chloride as catalyst. The column （4.6mm×250mm） packed by this resin wasapplied to the HPLC separation of scutellarin. Resolution, selectivity, column efficiency andretention time of separation of scutellarin were investigated to determine experimentalconditions, such as proportion of mobile phase, flow rate of mobile phase, column temperatureand sample concentration. The optimum conditions were as follows, the mobile phase wasacetonitrile：0.4% glacial acetic acid （27：73, v：v）, the flow rate was 1.0mL/min, columntemperature was 30℃, sample concentration was 300μg/mL. Under these conditions, the twocomponents were separated completely with the resolution was 2.20 and the retention time was7.7min. This study was helpful for large-scale preparation of scutellarin.

关 键 词：后交联 灯盏乙素 高效液相色谱 分离 

分 类 号：O647.3[理学—物理化学]