[关键词]
[摘要]
目的 建立指纹图谱和多指标定量的蜜远志质量评价方法。方法 Kromasil 100-5-C18色谱柱(250 mm×4.6 mm,5 μm)为固定相,以乙腈(A)-0.2%磷酸水溶液(B)为流动相进行梯度洗脱,体积流量为1.0 mL/min,检测波长318 nm。对16批蜜远志建立指纹图谱,确定共有峰并进行相似度分析结合化学计量学分析。采用Waters Xbridge Shiled RP C18色谱柱(250 mm×4.6 mm,5 μm)进行同时测定远志(口山)酮III、3,6'-二芥子酰基蔗糖、细叶远志皂苷、远志酸、远志皂苷元的含量。结果 在指纹图谱研究中,标定了27个共有峰,结合对照品和HPLC-Q-TOF-MS共指认8个成分,分别为西伯利亚远志糖A5、西伯利亚远志糖A6、远志(口山)酮IX、远志(口山)酮III、3,6'-二芥子酰基蔗糖、细叶远志皂苷、远志酸、远志皂苷元。聚类分析将16批样品分为3类;经主成分分析,主成分1~3是影响蜜远志质量评价的主要因子。多指标含量测定中远志(口山)酮III、3,6'-二芥子酰基蔗糖、细叶远志皂苷、远志酸、远志皂苷元的质量分数分别为0.027%~0.068%、0.074%~0.798%、1.1%~1.4%、0.15%~0.36%、0.15%~0.37%。经方法学验证,线性关系良好(r≥0.999 6),平均加样回收率为97.15%~100.9%。结论 所建立的指纹图谱结合多指标含量测定方法准确、高效,特征性强,可为蜜远志饮片的质量评价和临床应用提供有效参考。
[Key word]
[Abstract]
Objective To establish HPLC fingerprints and multi-components determination method of Miyuanzhi (honey-stir-baked Polygalae Radix). Methods Kromasil 100-5-C18 (250 mm×4.6 mm, 5 μm) column was used as stationary phase and acetonitrile-0.2% phosphoric acid aqueous solution was used as mobile phase for gradient elution, the flow rate was 1.0 mL/min and the detection wavelength was 318 nm. The fingerprints of 16 batches of Honey-stir-baked Polygalae Radix were established, the common peaks were determined, and the similarity analysis was carried out combined with stoichiometric analysis. The content of polygalaxanthone III, 3,6'-disinapoyl sucrose, tenuifolin, polygalacic acid and senegenin were determined simultaneously by Waters Xbridge Shiled RP C18. Results In the fingerprint study, 27 common peaks of Honey-stir-baked Polygalae Radix were demarcated and eight components were identified by reference and HPLC-Q-TOF-MS, which were sibiricose A5, sibiricose A6, polygalaxanthone IX, polygalaxanthone III, 3,6'-disinapoyl sucrose, tenuifolin, polygalacic acid and senegenin, respectively. The 16 batches of Honey-stir-baked Polygalae Radix were divided into three categories by cluster analysis. According to the principal component analysis, the principal components 1-3 were the main factors affecting the quality evaluation of the samples. The mass fractions of polygalaxanthone III, 3,6'-disinapoyl sucrose, tenuifolin, polygalacic acid and senegenin in multi-components determination were 0.027%-0.068%, 0.074%-0.798%, 1.1%-1.4%, 0.15%-0.36%, 0.15-0.37%, respectively. The method was verified, the linear relationship was good (r ≥ 0.999 6). The average recovery was 97.15%-100.9%. Conclusion The established HPLC fingerprints and multi-components determination method are accurate, efficient and characteristic, which can provide reference for the quality control and clinical application of Honey-stir-baked Polygalae Radix.
[中图分类号]
R286.2
[基金项目]
山东省重点研发计划重大科技创新工程项目(2021CXGC010511);山东省重点研发计划项目(2022CXGC010511);山东省重点研发计划项目(2021SFGC1202);济宁市重点研发计划(2022JNZC007);泉城产业领军人才支持计划创新团队项目(MRJT2105);“新高校20”项目科研带头人工作室(202228096)