摘 要

益心巴迪然吉布亚颗粒（以下简称益心颗粒）是由香青兰单味药经加工制成，用于神疲失眠，心烦气喘，神经衰弱等症的中药制剂，临床应用广泛。香青兰作为该制剂的关键组分，其质量的好坏直接影响其疗效。田蓟苷作为香青兰药材中主要活性成分，其含量的高低与益心颗粒的药效直接相关。且据文献报道^[1]田蓟苷作为指标成分在判别香青兰药材的真伪问题上具有较好的专属性，因此本课题选择田蓟苷为益心颗粒的质量指标进行研究。

本文旨在利用高效液相色谱法等技术建立益心颗粒中田蓟苷的鉴别方法和含量控制方法，并对所建立的方法进行验证，以达到对益心巴迪然吉布亚颗粒中田蓟苷定性和定量控制的目的。本实验分为两个部分，第一部分主要利用薄层色谱技术建立益心颗粒中田蓟苷的鉴别方法，并对所建立的方法进行验证。第二部分主要利用HPLC色谱技术建立益心颗粒中田蓟苷的含量测定方法，并对所建立的方法进行验证。实验结果表明，本次试验所建立的TLC法可以准确可靠地鉴别益心颗粒中田蓟苷，且专属性和重现性良好。本课题建立的益心颗粒中田蓟苷的含量测定方法，重复性（RSD为1.29%）及精密度（RSD为1.06%）良好，专属性强。结果表明本课题所建立的方法能准确的鉴别和控制益心颗粒中的田蓟苷含量，为检测和控制益心颗粒的质量提供了实验依据，对建立益心颗粒的质量标准具有重要意义。

关键词：香青兰、益心巴迪然吉布亚颗粒、田蓟苷、质量标准

Abstract

Yixin Badiranjibuya granules (hereinafter referred to as Yixin granules), which have been processed by fragrant blue scorpion, have been widely used in clinical practice.As the main active ingredient in the medicinal blue medicinal herb, the content of tilianin is directly related to the efficacy of Yixin Badiranjibuya granules. According to the literature, tilianin has good specificity as an indicator component. Therefore, the selection of scutellarin for the index component of Yixin Badiranjibuya granules was studied.

In this experiment, the TLC identification method and content determination method of tilianin in Yixin Badilan Jibuya Granules were established through the study of tilianin in Yixin Badilan Jibuya Granules, and the established method was validated to achieve the purpose of qualitative and quantitative control of thistleoside in Yixin Badilan Jibuya Granules.

The experiment was divided into two stages. The first stage was to identify the silymarin in Yixin granules by TLC and the second stage was to determine the content of silymarin in Yixin granules by high performance liquid chromatographyThe final experimental results of the first stage show that the TLC method established in this experiment can accurately and reliably identify thistleoside in Yixin granules, and has good specificity and reproducibility. In the second stage, the data of determination of thistleoside in Yixin Granules by HPLC established in this subject are RSD 1.29% for repetitive experiment, RSD 1.06% for precision experiment and good specificity.It indicated that the method can accurately determine the content of saponins in Yixin granules, and provide an experimental basis for the detection and control of the quality of saponins in Yixin granules, which is of great significance to the quality standard of Yixin granules.

Key words：Dracocephalum moldavica L、Yixin Badiran Gibiya Granules、Tilianin、Quality Standard

目 录

第一章 绪论..................................................................................................................1

1 香青兰研究概况........................................................................................................1

1.1 香青兰药理药效研究........................................................................................1

1.1.1 降血脂和抗动脉粥样硬化作用................................................................1

1.1.2 对缺血心肌和脑的保护作用....................................................................2

1.1.3 肿瘤抑制及免疫抑制作用........................................................................2

1.2 香青兰临床应用................................................................................................2

1.3 香青兰的化学成分............................................................................................3

1.3.1 挥发油化合物............................................................................................3

1.3.2 黄酮类化合物............................................................................................3

1.3.3 苯丙素类化合物........................................................................................4

1.3.4 三萜类与甾体类化合物............................................................................4

1.4 不同产地香青兰有效成分含量........................................................................4

2 田蓟苷研究概况........................................................................................................5

2.1 田蓟苷药理药效研究........................................................................................5

2.1.1 抗炎作用....................................................................................................5

2.2.2 抗肿瘤作用................................................................................................5

2.2.3 心肌缺血再灌注损伤的保护作用............................................................5

2.2 田蓟苷含量测定................................................................................................6

2.2.1 高效液相色谱法（HPLC法).....................................................................6

2.2.2 反向高效液相色谱法(RP-HPLC法）.......................................................6

2.2.3 紫外分光光度法（UV法）......................................................................6

2.2.4 含量测定法总结........................................................................................6

2.3 田蓟苷的分离....................................................................................................6

2.3.1 树脂分离法................................................................................................6

2.3.2 聚酰胺和硅胶色谱法................................................................................7

2.3.3 超声波分离法............................................................................................7

2.4 田蓟苷的纯化....................................................................................................7

2.4.1 柱色谱法....................................................................................................7

2.4.2 结晶法........................................................................................................7第二章 益心颗粒中田蓟苷的质量标准研究..............................................................8

1 益心颗粒中田蓟苷的薄层色谱鉴别........................................................................8

1.1 仪器和材料........................................................................................................8

1.2 益心颗粒中田蓟苷的薄层色谱鉴别方法........................................................9

1.2.1 薄层鉴别实验步骤....................................................................................9

1.2.2 专属性........................................................................................................9

1.2.3 重现性........................................................................................................9

2 高效液相色谱法含量测定益心颗粒中田蓟苷......................................................10

2.1 仪器与材料......................................................................................................10

2.2 益心颗粒中田蓟苷的含量测定方法..............................................................11

2.2.1 药材含量和转移率..................................................................................11

2.2.2 成品含量..................................................................................................11

2.2.3 方法建立和实验步骤..............................................................................11

2.2.4 方法验证..................................................................................................11

2.2.4.2 重复性验证......................................................................................11

2.2.4.2 精密度验证......................................................................................12

2.2.4.3 专属性验证......................................................................................12

3 结果与讨论..............................................................................................................12

参考文献......................................................................................................................15

附录..............................................................................................................................16

致谢..............................................................................................................................17

1. 绪论

1 香青兰研究概况

香青兰（Dracocephalum moldavica L），为唇形科一年生草本植物，具有香味，是我国多民族习用药材。香青兰在我国资源分布广泛，其主要生长于海拔220～1600m的干燥山地、山谷、河滩多石处。在国外也有广泛的分布，如苏联西伯利亚，东欧，西欧等地。