本文選題：松香基固定相　切入點(diǎn)：高效液相色譜　出處：《湖北民族學(xué)院》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：近年來,隨著石油資源的緊缺以及食品藥物安全問題的日益突出,人們逐漸著眼于可再生、綠色環(huán)保、廉價(jià)易得的材料。其中,松香作為天然無毒的原料,其獨(dú)特的菲環(huán)結(jié)構(gòu)和較好的力學(xué)剛性吸引了大量研究者的目光。本文采用天然松香改性的交聯(lián)劑,合成松香基高效液相色譜固定相,用于分離天麻素(Gastrodin)及其衍生物,主要內(nèi)容如下:1.制備了Ru131、Ru232松香基高分子微球及其酯化修飾的Ru131松香基高分子微球,采用激光粒度測(cè)定儀、比表面積及氮?dú)馕絻x、熱重分析儀對(duì)合成的微球進(jìn)行表征。結(jié)果表明:松香基高分子微球粒徑主要分布在3~8μm范圍內(nèi),球型非常好,具有較為豐富的孔結(jié)構(gòu),且在25~300℃溫度范圍內(nèi)熱穩(wěn)定性良好。2.分別采用甲醇、乙二醇、甘油和葡萄糖修飾Ru131色譜柱(分別命名為:Ru131-Mt、Ru131-Et、Ru131-Gly、Ru131-Glu色譜柱),分離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),并探索了乙酸濃度、流速、柱溫對(duì)甲醇修飾的Ru131色譜柱對(duì)Gastrodin和Methylarbutin分離效果的影響,結(jié)果表明,甲醇修飾的Ru131色譜柱對(duì)兩組競(jìng)爭(zhēng)分子分離效果最好,在25℃,流速0.3 m L/min,甲醇為流動(dòng)相條件下,Gastrodin和Methylarbutin分離度最高,Rs為2.30。3.通過Ru232松香基高分子色譜柱分離Gastrodin及其衍生物Methylarbutin和Phenolglucoside,考察了乙腈濃度、乙酸濃度、流速、柱溫對(duì)分離效果的影響,結(jié)果表明Ru232色譜柱對(duì)2組競(jìng)爭(zhēng)分子分離效果良好;在25℃,流速0.3 m L/min,0.05%乙酸甲醇為流動(dòng)相條件下,Gastrodin與衍生物Phenolglucoside和Methylarbutin分離度最高,Rs分別為1.54和2.73;通過范特霍夫方程,計(jì)算出2組競(jìng)爭(zhēng)分子的ΔH、ΔS、ΔG熱力學(xué)數(shù)據(jù),并對(duì)其分離進(jìn)行理論分析。4.將Ru232松香基高分子色譜柱分離純化天麻水提物,分離純化后的Gastrodin純度達(dá)到82%,說明該填料能夠有效的分離純化Gastrodin,具備應(yīng)用價(jià)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，

本文編號(hào)：1566171