毕业设计（论文）-高效液相色谱法对样品的分离与纯化精选.docVIP

高效液相色谱法 对样品A的分离与纯化 目 录 摘要 I Abstract II 引 言 1 第1章 绪论 2 1.1高效液相色谱简介 2 1.1.1正相色谱和反相色谱 2 1.1.2制备色谱的概况 3 1.2高效液相色谱柱选择与使用 6 1.2.1色谱分离模式的选择 6 1.2.2制备型高效液相色谱柱 7 第2章 样品中杂质的分离与纯化 9 2.1实验仪器 9 2.2实验试剂 9 2.3实验步骤 9 第3章 结果与讨论 18 结 论 19 致 谢 20 参考文献 21 高效液相色谱法对样品A的分离与纯化 摘要：高效液相色谱作为一种重要的分析方法，广泛的应用于化学和生物化学中、医药品、化学、环保、生命科学和食品工业的研究上。本论文采用反相高效制备液相色谱对样品A进行了分离，纯化和制备。在样品的制备过程中，对流动相、洗脱梯度、进样量、色谱柱的种类等制备条件进行了优化。优化出制备条件后，使用制备型高效液相色谱对样品进行分离纯化，收集大量样品目标峰的馏分，进行减压蒸馏和冷冻干燥后，得到干燥的样品。经LC-MS检测，其纯度仅有89.733%。通过对液相色谱分离条件的再次优化，经过多次的制备分离，对样品进行富集。经LC-MS检测，最终纯度达到了100%。该方法操作简单，方便，安全性强，污染性小，检测限低。 关键词: 高效液相色谱 反相 分离 制备 Separation and Purification of Compound A by High Performance Liquid Chromatography Abstract: High performance liquid chromatography as an important analytical method, widely used in chemical and biochemical, medicine, chemical, environmental protection, life sciences, and food industry research. The samples were separated, purified and prepared by reversed phase high performance liquid chromatography. In the preparation of the sample, the preparation method was screened, including the mobile phase, the elution gradient, the injection volume, the type of column and so on. After the preparation conditions were optimized, the samples were separated and purified by preparative high performance liquid chromatography, and the fractions of the target peaks were collected. After vacuum distillation and freeze drying, the dried samples were obtained. The purity was only 89.733% by LC-MS analyze. The sample was enriched by re-optimization of the separation conditions of the liquid chromatography and by several preparative separations. By LC-MS detection, the final purity is 100%. The method is simple, convenient, high safety, less pollution, low detection limit. Key words: high performance liquid chromatography; reverse phase; separation; preparation 引 言 制备型高效色谱是利用“吸附-洗脱”的原理进行分离纯化。在国外已有多年的发展，而在我国只是在20世纪90年代末期才渐渐开始普及。近年来，随着生物化学，有机化学，制药行业等相关行业的快速发展，制备型高效液相色谱已经越来越广泛的被应用在相关项目和产品的产业化之中。 随着高效液相色谱的快速发展，出