不同厂家一清颗粒UPLC指纹图谱的比较

Study on UPLC Fingerprint of Yiqing Granules from Different Manufacturers

摘要: 目的：建立不同厂家不同批次一清颗粒UPLC指纹图谱分析方法，比较不同厂家之间指纹图谱的差异，为有效控制及质量评价不同厂家一清颗粒的质量提供有力依据。方法：采用ZORBAX RRHD Eclipse Plus C18 (2.1 × 100 mm, 1.8 μm)色谱柱，乙腈(A)-0.1%的甲酸水溶液(B)为流动相，梯度洗脱，检测波长为254 nm；流速为0.1 ml/min；柱温为30℃；进样量为1 μl。测定24批不同厂家的一清颗粒的指纹图谱，并对其结果进行相似度、系统聚类和主成分分析。同时对一清颗粒中的部分化学成分进行指认。结果：24批样品UPLC指纹图谱相似度在0.674~0.978之间，不同厂家一清颗粒成分存在差异，同一厂家一清颗粒质量较稳定。系统聚类分析将24批一清颗粒分为3大类，同一厂家之间聚为一类。且利用VIP值筛选出6个导致差异性的差异峰。同时指认出了大黄素、大黄酸、大黄酚、芦荟大黄素、大黄素甲醚、黄芩苷、黄芩素、汉黄芩素、盐酸小檗碱、巴马汀等10个化学成分。结论：该方法简单、可靠、重复性及稳定性好，适用于不同厂家一清颗粒的质量控制。

Abstract: Objective: To establish a UPLC fingerprint analysis method for Yiqing granules of different batches from different manufacturers, compare the differences in fingerprints between different manufac-turers, and provide a strong basis for effective control and quality evaluation of Yiqing granules produced by different manufacturers. Methods: ZORBAX RRHD Eclipse Plus C18 (2.1 × 100 mm, 1.8 μm) column was used with acetonitrile (A)-0.1% formic acid aqueous solution (B) as mobile phase. The detection wavelength was set at 254 nm. The flow rate was 0.1 mL/min. The column tempera-ture is 30˚C. The injection volume was 1 μL. The fingerprints of 24 batches of Yiqing granules from different manufacturers were determined, and the similarity comparison, cluster analysis and principal component analysis of Yiqing granules from different manufacturers were carried out. At the same time, some chemical constituents in Yiqing granules were identified. Results: The similarity of the UPLC fingerprint of 24 batches of samples was between 0.674 and 0.978. There were differences in the composition of Yiqing granules from different manufacturers. The quality of Yiqing granules from the same manufacturer was stable. Systematic cluster analysis divided 24 batches of Yiqing granules into three categories, and the same manufacturers were clustered into one category. The VIP value was used to screen out six differential peaks leading to differences. At the same time, ten chemical components were identified, including emodin, rhein, chrysophanol, aloe-emodin, emodin methyl ether, baicalin, baicalein, wogonin, berberine hydrochloride, palmatine, etc. Conclusion: The method is simple, reliable, reproducible and stable, which is suitable for the quality control of Yiqing granules from different manufacturers.