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目的建立香砂六君丸的HPLC指纹图谱,考察不同厂家不同批次香砂六君丸质量的一致性,为完善该制剂的质量评价体系奠定基础。方法采用HPLC法进行测定,Sepax Bio-C18(250 mm×4.6 mm,5μm)色谱柱,乙腈-0.1%醋酸水溶液梯度洗脱,检测波长260 nm,体积流量1.0 m L/min,柱温30℃,对所得各样品的指纹图谱进行整体相似度计算,并对其共有色谱峰峰面积进行聚类分析。结果首次建立了香砂六君丸的HPLC指纹图谱,标定共有峰17个,分别确定了其归属药材,并通过对照品对照、UPLC-Q-TOF-MS鉴定了16个色谱峰的化学成分。16家生产企业49批次样品的指纹图谱相似度分布在0.617~0.988,通过聚类分析大致可聚为4类。结论市售香砂六君丸的质量参差不齐,不同厂家样品的质量差异较大。该方法简便、可靠,可用于香砂六君丸的质量评价,为进一步完善香砂六君丸的质量标准提供参考。
OBJECTIVE To establish the HPLC fingerprint of Xiangsha Liujun pill and investigate the consistency of the quality of Xiangsha Liujun pill in different batches of different manufacturers so as to lay the foundation for improving the quality evaluation system of this preparation. Methods The HPLC method was used for the determination. The separation was performed on a Sepax Bio-C18 column (250 mm × 4.6 mm, 5 μm) with gradient elution of acetonitrile and 0.1% acetic acid. The detection wavelength was 260 nm and the volume flow rate was 1.0 m L / , The fingerprint of each sample was calculated for the overall similarity, and its peak area of common chromatographic clustering analysis. Results The HPLC fingerprint of Xiangsha Liujun pill was established for the first time. The total number of peaks was 17 and its own medicinal materials were identified. The chemical constituents of 16 peaks were identified by UPLC-Q-TOF-MS. Fingerprint similarity of samples from 49 batches of 16 manufacturing enterprises ranged from 0.617 to 0.988 and clustered into 4 categories by cluster analysis. Conclusion The quality of Xinshaliu Jun pill is uneven, and the quality of samples from different manufacturers is quite different. The method is simple and reliable, which can be used for the quality evaluation of Xiangsha Liujun pill and provide a reference for further improving the quality standard of Xiangsha Liujun pill.