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星夏止痛贴膏化学成分快速分析及指纹图谱研究

Rapid analysis of chemical component and fingerprint research of Xingxia Zhitong Plaster

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【作者】 潘林平陈国成王小艳毕晓黎卢文森谢灿辉胥爱丽

【Author】 PAN Linping;CHEN Guocheng;WANG Xiaoyan;BI Xiaoli;LU Wensen;XIE Canhui;XU Aili;Guangzhou Yuexiu District Traditional Chinese Medicine Hospital;Guangdong Province Engineering Technology Research Institute of T.C.M;The Fifth Clinical School of Guangzhou University of Traditional Chinese Medicine;

【通讯作者】 胥爱丽;

【机构】 广州市越秀区中医医院广东省中医药工程技术研究院广州中医药大学第五临床医学院

【摘要】 目的 建立星夏止痛贴膏化学成分的快速分析方法及指纹图谱。方法 采用超高效液相色谱-飞行时间串联质谱联用(UPLC-Q-TOF-MS/MS)法,以Waters ACquity Uplc Beh C18柱(100 mm×2.1 mm,1.7μm)为色谱柱,以乙腈-0.1%甲酸为流动相进行梯度洗脱;流速:0.25 mL/min,柱温:35℃。电喷雾离子源(ESI)在正、负离子模式下采集数据,通过分析各成分的精确质荷比和二级碎片离子信息,并结合质谱数据库信息、对照品的保留时间和文献报道,对其碎片离子的裂解规律进行匹配,快速鉴定星夏止痛贴膏的化学成分,通过高效液相色谱(HPLC)法建立制剂的指纹图谱。结果 共鉴别出68种成分,包括生物碱类25种、苯丙素类12种、黄酮类9种、萜类7种、蒽醌类4种、有机酸类6种、挥发油类1种、甾体类1种、酚类2种和氨基酸类1种,指纹图谱共确定13个共有峰特征峰,10批样品的相似度均大于0.90。结论 本方法快速地鉴定了星夏止痛贴膏中的主要化学成分并建立了指纹图谱,为该制剂的深入开发利用奠定了基础。

【Abstract】 Objective To establish a method for rapid analysis of chemical components and Fingerprint in Xingxia Zhitong Plaster. Methods An ultra performance liquid chromatography tandem quadrupole time-of-flight mass spectrometric method(UPLC-Q-TOF-MS) was used. The analysis was performed on Waters ACQUITY UPLC BEH C18(100 mm × 2.1 mm,1.7 μm)column with a mobile phase consisting of 0.1% formic acid and acetonitrile in a gradient mode. The flow rate was set at 0.25 mL/min and the column temperature was maintained at 35 ℃. ESI ion source was used to ensure the data collected in positive and negative ion mode. By analyzing the precise mass to charge ratio and secondary fragment ion information of each component, the chemical components of Xingxia Zhitong plaster were identified by comparing with the retention time and the mass data of the reference substances,and consulting literature reports and mass spectrometry database. The fingerprints of preparation were established by high performance liquid chromatography(HPLC) method. Results 68 compounds were identified by the time of flight mass spectrometry and literature data, including 25 alkaloids, 12 phenylpropanoids, 9 flavonoids, 7 terpenoids, 4 anthraquinones, 6 organic acids, 1 volatile oil, 1 steroid, 2 phenols and 1 Amino acid, respectively. A total of 13 common peaks were identified,the similarity of the 10 batches was greater than 0.90. Conclusion This method quickly identified the main chemical components in Xingxia Zhitong Plaster and established a fingerprint spectrum, laying the foundation for the further development and utilization of the formulation.

【基金】 广州市中医药临床核心和特色诊疗技术项目(穗卫中医[2022]7号)
  • 【文献出处】 广东药科大学学报 ,Journal of Guangdong Pharmaceutical University , 编辑部邮箱 ,2025年05期
  • 【分类号】R286.0
  • 【下载频次】32
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