[关键词]
[摘要]
目的 建立加味黄芪桂枝五物汤(Jiawei Huangqi Guizhi Wuwu Decoction,JHD)HPLC指纹图谱,鉴定其主要化学成分,并阐明指纹图谱共有峰的成分归属。方法 HPLC指纹图谱检测采用Hypersil ODS色谱柱(250 mm×4.6 mm,5 μm);流动相为乙腈-0.2%甲酸水溶液,梯度洗脱,体积流量1 mL/min,检测波长为250 nm,柱温为30℃;运用“中药色谱指纹图谱相似度评价系统”进行相似度评价,并以高效液相色谱串联四级杆飞行时间质谱(liquid chromatography-quadrupole time-of-flight mass spectrometry,LC-Q-TOF/MS)方法对指纹图谱中化学成分进行分析,通过对照品、化合物质谱信息结合文献报道鉴定其结构,进一步通过药材指纹图谱阐明共有峰的成分归属。结果 建立了JHD的HPLC指纹图谱,确定了20个共有峰,10批样品相似度为0.920~0.990。在此基础上共鉴定出JHD中70个化学成分,包括28个黄酮类、23个三萜类、5个单萜苷类、5个有机酸类、5个姜辣素类及4个其他类化合物。结论 HPLC指纹图谱结合LC-Q-TOF/MS定性鉴别,能够体现JHD组分的整体特征,可为其质量控制研究奠定基础。
[Key word]
[Abstract]
Objective To establish the HPLC fingerprint of Jiawei Huangqi Guizhi Wuwu Decoction (加味黄芪桂枝五物汤, JHD), identify its main chemical components, and clarify the components of the common peaks of the fingerprint. Methods A Hypersil ODS column (250 mm×4.6 mm, 5 μm) was selected for HPLC fingerprint, acetonitrile and 0.2% formic acid aqueous solution was used as the mobile phase in a gradient elution. The mobile phase was set at a flow rate of 1.0 mL/min. The detection wavelength was set at 250 nm and the column temperature was 30 ℃. The “Similarity Evaluation System for Chromatographic Fingerprint of TCM” was used to evaluate the similarity of the HPLC fingerprints of samples. The chemical components in the fingerprint were analyzed by the liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-Q-TOF/MS). The structure was identified by comparison with standards and mass spectrum information reported in the literature. Then, the origin of ingredients was clarified by combining the fingerprints of single medicinal material. Results The HPLC fingerprints were established with 20 common peaks obtained. The similarity of 10 batches of samples was 0.920—0.990. Seventy components of JHD were identified, including 28 flavonoids, 23 pentacyclic triterpene saponins, 5 monoterpene glycosides, 5 organic acids, 5 gingerols and 4 other kinds of compounds. Conclusion HPLC fingerprint binding LC-Q-TOF/MS qualitative identification reflects the overall characteristics of JHD. It can lay the foundation for its quality control study.
[中图分类号]
R284.1
[基金项目]
重大新药创制科技重大专项(2019ZX09301145)