摘要
本研究主旨在于南方菟丝子缠绕茎中金丝桃苷对照品的制备以及含量测定方法的建立。首先,采用AB-8大孔吸附树脂富集南方菟丝子总黄酮,再用聚酰胺柱色谱富集黄酮苷,采用Sephadex LH-20凝胶柱从黄酮苷中分离金丝桃苷单体,并采用紫外光谱(UV)、红外光谱(IR)、质谱(MS)以及核磁共振氢谱(~1H-NMR)、核磁共振碳谱(^(13)C-NMR)等波谱技术进行结构鉴定,利用薄层色谱法(TLC)、高效液相色谱法(HPLC)、高效液相色谱-质谱联用技术(HPLC-MS)等方法进行纯度测定,测得其质量分数大于99.0%;南方菟丝子茎中金丝桃苷的含量测定则采用反相高效液相色谱法(RP-HPLC),结果显示,金丝桃苷在1.47~7.36μg/m L范围内呈良好线性关系(R^2=0.999 5),平均回收率为104.5%,RSD为2.36%(n=5)。本法得到的金丝桃苷对照品符合中药化学对照品的相关技术要求,可用于含金丝桃苷相关植物药及制剂的质量控制。含量测定方法准确、简便、可靠和重复性好。
The aim o f this study was to establish methods for the preparation and determination of hyperin reference substance from the stem of Cuscuta australis.Firstly,the total flavonoids of the stem of Cuscuta australis was enriched and purified with AB-8 macroporous resin.Then flavonoid glycoside was enriched by polyamide and hyperin monomer was separated by sephadex LH-20 column chromatography.The structure of hyperin was demonstrated by UV,IR,MS,1H-NMR and 13C-NMR spectral analysis.The purity of hyperin was determined by TLC,HPLC and HPLC-MS,of which the purity of hyperin was higher than 99.0%.A reversed-phase HPLC method for detecting the content of hyperin was also established.Results showed that hyperin was successfully separated from the stem of Cuscuta australis.There was a good linearity within the range of 1.477.36 μg/m L（R2=0.999 5）.The average recovery was 104.5% and RSD was 2.36%（n=5）.It could be concluded that the obtained hyperin reference substance could be used as the chemical reference substance for controlling the quality of related medicinal preparations.The quantitative analysis method was accurate and simple with good reproducibility.
出处
《分子植物育种》
CAS
CSCD
北大核心
2018年第1期234-239,共6页
Molecular Plant Breeding
基金
福建省教育厅中青年教师教育科研项目(JAT170705)
厦门医学院自然科学类项目(K2016-19
K2016-37
Z0902)共同资助
作者简介
通讯作者:张岗.zg@xmmc.edu.cn
