不同厂家香砂六君丸的HPLC指纹图谱研究

HPLC fingerprint of Xiangsha Liujun Pills from different manufacturers

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 mL/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 an HPLC fingerprint of Xiangsha Liujun Pills（XLP）, and to apply this method to determining 49 batches of samples from 16 different manufacturers for quality evaluation, supporting the foundation of quality control system of XLP. Methods The HPLC separation was performed on a Sepax Bio-C18 reversed-phase column in gradient mode of acetonitrile-0.1% acetic acid with UV detection at 260 nm. The column temperature was kept at 30 ℃, and the flow rate of mobile phase was 1.0 m L/min. The fingerprint similarities and cluster analysis based on the chromatographic peaks in detected samples were obtained. Results The HPLC fingerprint of XLP was developed firstly. Seventeen common fingerprint peaks were indicated and attributed to raw materials, and 16 of them were identified by comparison with reference standards and UPLC-Q-TOF-MS. The analyzed samples were geographically classified into four classes with the similarities between 0.617—0.988. Conclusion Significant differences of quality in XLP on the market are observed. The method is simple, reliable, and suitable for the quality control of XLP, supplying helpful information for the comprehensive evaluation of XLP.