一清颗粒HPLC指纹图谱研究

Study on the HPLC Fingerprint of Yiqing Granules

目的:建立一清颗粒的HPLC指纹图谱分析方法,为评价其质量提供依据。方法:采用Agilent ZORBAX SB-C_(18)色谱柱(250 mm×4.6 mm,5μm),以乙腈(A)-0.2%磷酸水溶液(用三乙胺调节pH至3.0,B)为流动相,梯度洗脱(0~5 min,10%A→20%;5~20 min,20%A→30%A;20~25 min,30%A→45%A;25~35 min,45%A;35~45 min,45%A→80%A;45~50 min,80%A),流速:1.0 ml·min^(-1),检测波长:254 nm,柱温:35℃;采用HPLC法测定12批一清颗粒的指纹图谱,建立指纹图谱共有模式。结果:12批一清颗粒指纹图谱标定了共有峰22个,指认了其中7个化学成分。12批样品指纹图谱与对照指纹图谱的相似度均大于0.990。结论:所建立的方法准确、可行,可用于一清颗粒质量控制。

Objective： To establish an HPLC fingerprint of Yiqing granules to provide reference for the effective quality control. Methods： The analysis was carried out on an analytical Agilent ZORBAX SB-C18 （250 mm × 4.6 mm,5 μ）column with gradient elntion by acetonitrile（ A）- 0.2% phosphoric acid solution（ adjusting pH to 3.0 with triethylamine, B） （0-5 min： 10% A →20% ;5-20 min： 20% A→30% A; 20-25 min： 30% A→45% A; 25-35 min： 45% A; 35-45 min： 45% A→80% A; 45-50 min： 80% A）at the detection wavelength of 254 nm and the flow rate of 1.0 ml · min-1 , and the column temperature was 35 ℃. Twelve batches of Yiqing granules were determined by HPLC and a common mode of fingerprint was established. Results： There were 22 common peaks in the fingerprints of the twelve batches of Yiqing granules,and seven of them were identified. The similarities of fingerprints of the twelve batches of Yiqing granules were over 0. 990 suggesting good reproducibility. Conclusion： The developed method is accurate and feasible, and can be used for the quality control of Yiqing granules.