中国药物警戒 ›› 2026, Vol. 23 ›› Issue (1): 83-87.
DOI: 10.19803/j.1672-8629.20250400

• 基础与临床研究 • 上一篇    下一篇

基于1H-NMR和LC-MS的普乐安片相似度分析及山柰酚含量测定

蔡尚佐1, 诸葛慧2, 唐宇2, 王毅1,*   

  1. 1杭州医学院药学院,浙江 杭州 310013;
    2浙江大学药学院,浙江 杭州 310058
  • 收稿日期:2025-06-18 出版日期:2026-01-15 发布日期:2026-01-15
  • 通讯作者: *王毅,男,博士,教授,中药分析与质量标准。E-mail: zjuwangyi@zju.edu.cn
  • 作者简介:蔡尚佐,男,在读硕士,中药分析。
  • 基金资助:
    国家自然科学基金资助项目（82204614）; 中央高校基本科研业务费专项资金资助项目（226-2024-00001）

Consistency Evaluation and Kaempferol Content Determination of Multiple Batches of Pule’an Tablets Based on 1H-NMR and LC-MS

CAI Shangzuo1, ZHU Gehui2, TANG Yu2, WANG Yi1,*   

  1. 1School of Pharmacy, Hangzhou Medical College, Hangzhou Zhejiang 310013, China;
    2College of Pharmaceutical Sciences, Zhejiang University, Hangzhou Zhejiang 310058, China
  • Received:2025-06-18 Online:2026-01-15 Published:2026-01-15

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摘要： 目的 探究普乐安片相似度及其指标性成分山柰酚的含量,为普乐安片的质量分析提供参考。方法 用70%乙醇提取普乐安片,旋蒸除醇后分别使用石油醚和乙酸乙酯进行萃取,后运用定量核磁共振氢谱（1H-NMR）和液相色谱-质谱联用（LC-MS）2种分析技术对9批药品乙酸乙酯萃取部分进行波谱数据采集。利用夹角余弦法对预处理后的数据进行计算评估其相似度。选择3,5-二硝基苯甲酸甲酯作为内标,通过定量核磁内标法对普乐安片中的山柰酚成分进行定量分析。结果 9批次普乐安片的1H-NMR图谱相似度为0.984,LC-MS图谱的相似度为0.987。采用此实验中的核磁定量内标法,测得本实验室制备该样品中山柰酚的含量为每片2.03~12.86 mg。结论 不同批次间普乐安片相似度较高,为药效和用药安全提供了保障。定量核磁内标法操作便捷、快速准确,为山柰酚的含量测定提供参考。

关键词: 普乐安片, 山柰酚, 3,5-二硝基苯甲酸甲酯, 核磁共振氢谱, 液相色谱-质谱联用, 夹角余弦法

Abstract: Objective To investigate the similarity of Pule’an tablets and the content of their marker compound, kaempferol. Methods The tablets were extracted with 70% ethanol before being concentrated under reduced pressure to afford crude extracts (CRs) that were then extracted with petroleum ether and ethyl acetate (EA) respectively. The analytical data including quantitative 1H-NMR and LC-MS of the extract portion EA was collected. In order to find out about the batch-to-batch consistency of the samples, the cosine similarity calculation method was used to calculate the pre-processed data. Methyl 3,5-dinitrobenzoate was selected as the internal calibrant (IC) to calculate the content of kaempferol in Pule’an tablets using the qNMR method. Results The 1H-NMR similarity of the 9 batches of Pule’an tablets was determined to be 0.984, while LC-MS similarity was 0.987. Using the internal calibration method of quantitative NMR, the content of kaempferol in the samples was measured to range from 2.03 mg to 12.86 mg per tablet. Conclusion The results suggest that the similarity between the 9 batches of Pule’an tablets is high, which can help guarantee the efficacy and safety of the product. The IC-qHNMR method used for content determination of kaempferol is user-friendly, fast, and accurate.

Key words: Pule’an Tablets, Kaempferol, Methyl 3,5-Dinitrobenzoate, 1H-NMR, LC-MS, Cosine Similarity

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