摘要本方案目的在于,建立一套基质微固相分散萃取(TMSPD)技术,并且结合超高效液相色谱(UPLC),从而对陈皮中的黄酮类有效成分进行分析测定,通过考察影响实验的各种因素包括分散剂种类、样品和分散剂的质量比、研磨时间、洗脱液种类和体积、加水的影响、辅助吸附剂的影响、洗脱液pH,并且可以使实验中所用的材料得到(样品、吸附剂、洗脱液)最小化,同时也契合了绿色化学的概念。为了能够得到最优的效果,我们将研磨时间规定为150s,使用SBA-15(不含共吸附剂与水)作为吸附剂,且规定未添加乙酸的500μl的甲醇为洗脱溶剂,样品与吸附剂基质的质量比为1:1。从而能够在最后建立方法进行样品真实含量的测定,该方法灵敏度高,选择性好,应用前景良好。在最优条件下,实验有一个较宽的线性范围0.1-100 ng。与此同时,该方法在对植物样品总黄酮测定中给出了令人满意的回收率90-101%。结果表明,该实验方法对陈皮进行样品制备和目标化合物分析方面具有非常大的发展空间。44043
ABSTRACT The program aims to establish a set of matrix micro dispersive solid phase extraction (TMSPD) technology, and combined with ultra high-performance liquid chromatography (UPLC), thus Citrus flavonoids active ingredients Determination by systemic experiments to examine the impact variety of factors including the type of dispersant, the mass ratio of the sample and dispersant, grinding time, type and volume of the eluent, water impact, the impact of the auxiliary adsorbent, the eluent pH, and allows the material used in the experiment get (samples, adsorbents, eluent) minimized while also fit the concept of green chemistry. In order to obtain the best results, we require the grinding time is 150s, using SBA-15 as an adsorbent, and the provision of an elution solvent of acetic acid was not added 500μl of methanol, the mass ratio of the matrix of the sample with the adsorbent is 1: 1 , with no water co-adsorbent case. Thus enabling the establishment of the final sample was measured for the real content, the method of high sensitivity, good selectivity and good prospects. Under optimal conditions, the experimental linear over a wide range 0.1-100 ng. At the same time, the method for the determination of total flavonoids in plant samples gives satisfactory recovery of 90-101%. The results show that the experimental method to analyze aspects of Citrus target compound sample preparation and has a very large space for development
毕业论文关键词:基质固相提取; 黄酮; 离子液; 陈皮; 超高效液相色谱
Keyword: Matrix solid-phase dispersion; Flavone; Ionic liquids; Dried tangerine peel;Ultra-performance liquid chromatography
目 录
第一章 引言 4
1.1陈皮的概论 4
1.2微萃取概论 4
1.3分子筛概论 5
1.4基质固相分散概论 5
第二章 实验部分 6
2.1 仪器与试药 6
2.2 仪器条件 6
2.3样品制备和提取 6
2.3.1 索氏提取 6
2.3.2 MSPD流程 7
2.4 分子筛合成过程 7
2.5 优化考察过程 8
2.5.1 吸附剂种类考察 8
2.5.2 样品和吸附剂之间比例考察