摘要在本文中，我们使用一种新型高效的提取方法：基质微固相提取（TMSPD），同时结合超高效液相色谱（UPLC）对枳壳中两种黄酮类成分（新橙皮苷和柚皮苷）进行提取和检测。通过设计实验对离子液种类、浓度、体积，吸附剂种类，样品和吸附剂之间比例，研磨时间，洗脱液种类等几个参数进行优化，取得最优实验条件为使用弗罗里硅土（150mg）作为吸附剂，1-丁基-3-甲基咪唑四氟硼酸盐（0.4mL，250mm）作洗脱溶剂。这项研究首次尝试在基质固相提取中使用一种绿色安全的洗脱剂：离子液（ILs）解吸化合物。此外，相比较中国药典中记载的方法，该方法在提高富集因子、减少试剂消耗和环境污染方面具有一些优点。在最优条件下，实验有一个较宽的线性范围0.25-10ng，r2 值为1.00。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95-101%。识别两种分析物的检测限在0.05到0.06 ng之间。结果表明，该优化方法在对复杂的中草药样品进行样品制备和目标化合物分析方面具有很大潜力。46734

ABSTRACT

  In this article, two flavonoids (neohesperidin and naringin) in Fructus Aurantii were effectively and selectively extracted by trace of matrix solid phase dispersion (TMSPD) method, followed by ultra-performance liquid chromatography-ultraviolet detection. Several parameters, such as type of elution solvents, concentration of ILs, the mass ratio of sample to sorbent, grinding time and type of dispersant, were optimized to improve the performance of the method through the experimental design. The best results were obtained using Florisil (150mg) as sorbents and 1-butyl-3-methylimidazolium tetrafluoroborate (0.4 mL, 250mM) as elution solvent. This work presented the first attempt of using ionic liquids as a green eluting solvent for desorption of the investigated compounds in TMSPD. Moreover, compared with the pharmacopoeia method, the proposed method has some advantages in improving the enrichment factor, reducing consumption of reagents and environment pollution. A wide linear range of 0.25-10 ng was observed with r2 values of 1.00. Meanwhile, the method gave acceptable recoveries (95-101%) for determination of flavonoids in plant samples. The limits of detection for identification of two analytes ranged between 0.05 and 0.06 ng. The results showed that the optimized method has great potential for sample preparation in routine analysis of target components in complex herbal samples.

毕业论文关键词：黄酮; 枳壳; 离子液; 基质固相提取

Keyword: Flavonoids；Fructus Aurantii；Ionic liquids；Matrix solid-phase dispersion

目    录

第一章 引言 5

1.1 枳壳概论 5

1.2 基质固相提取概论 6

1.3 离子液概论 7

第二章 实验部分 9

2.1 仪器与试药 9

2.2 色谱条件 10

2.3 对照品溶液制备过程 10

2.4 供试品溶液的制备 10

2.5 基质微固相分散萃取步骤 10

2.6 离子液种类考察 11

2.7 离子液浓度考察 11

2.8 离子液体积考察 11

2.9 吸附剂种类考察 12

2.10 药材和吸附剂比例考察 12

2.11 研磨时间考察 12

2.12 标准曲线绘制