松香基高效液相色谱固定相的制备及对天麻素的分离研究

发布时间：2018-03-04 15:13

  本文选题：松香基固定相　切入点：高效液相色谱　出处：《湖北民族学院》2017年硕士论文　论文类型：学位论文

【摘要】：近年来,随着石油资源的紧缺以及食品药物安全问题的日益突出,人们逐渐着眼于可再生、绿色环保、廉价易得的材料。其中,松香作为天然无毒的原料,其独特的菲环结构和较好的力学刚性吸引了大量研究者的目光。本文采用天然松香改性的交联剂,合成松香基高效液相色谱固定相,用于分离天麻素(Gastrodin)及其衍生物,主要内容如下:1.制备了Ru131、Ru232松香基高分子微球及其酯化修饰的Ru131松香基高分子微球,采用激光粒度测定仪、比表面积及氮气吸附仪、热重分析仪对合成的微球进行表征。结果表明:松香基高分子微球粒径主要分布在3~8μm范围内,球型非常好,具有较为丰富的孔结构,且在25~300℃温度范围内热稳定性良好。2.分别采用甲醇、乙二醇、甘油和葡萄糖修饰Ru131色谱柱(分别命名为:Ru131-Mt、Ru131-Et、Ru131-Gly、Ru131-Glu色谱柱),分离Gastrodin及其衍生物:苯基β-D-吡喃葡萄糖苷(Phenolglucoside)和4-甲氧基苯基-β-D-吡喃葡萄糖苷(Methylarbutin),并探索了乙酸浓度、流速、柱温对甲醇修饰的Ru131色谱柱对Gastrodin和Methylarbutin分离效果的影响,结果表明,甲醇修饰的Ru131色谱柱对两组竞争分子分离效果最好,在25℃,流速0.3 m L/min,甲醇为流动相条件下,Gastrodin和Methylarbutin分离度最高,Rs为2.30。3.通过Ru232松香基高分子色谱柱分离Gastrodin及其衍生物Methylarbutin和Phenolglucoside,考察了乙腈浓度、乙酸浓度、流速、柱温对分离效果的影响,结果表明Ru232色谱柱对2组竞争分子分离效果良好;在25℃,流速0.3 m L/min,0.05%乙酸甲醇为流动相条件下,Gastrodin与衍生物Phenolglucoside和Methylarbutin分离度最高,Rs分别为1.54和2.73;通过范特霍夫方程,计算出2组竞争分子的ΔH、ΔS、ΔG热力学数据,并对其分离进行理论分析。4.将Ru232松香基高分子色谱柱分离纯化天麻水提物,分离纯化后的Gastrodin纯度达到82%,说明该填料能够有效的分离纯化Gastrodin,具备应用价值。
[Abstract]:In recent years, with the shortage of petroleum resources and the increasingly prominent problem of food and drug safety, people are gradually focusing on renewable, green, cheap and easily available materials. Among them, rosin is a natural non-toxic raw material. Its unique phenanthrene ring structure and good mechanical rigidity have attracted the attention of many researchers. In this paper, rosin based high performance liquid chromatographic stationary phase was synthesized by using natural rosin modified crosslinking agent for the separation of Gastrodinin and its derivatives. The main contents are as follows: 1. Ru131- Ru232 rosin based polymer microspheres and Ru131 rosin based polymer microspheres modified by esterification were prepared. The laser particle size measurement, specific surface area and nitrogen adsorption instrument were used. The synthesized microspheres were characterized by thermogravimetric analysis. The results showed that the diameter of rosin based polymer microspheres was mainly distributed in the range of 3 渭 m, the spherical shape was very good, and the microspheres had abundant pore structure. And the thermal stability is good in the temperature range of 25 鈩，

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