基于指纹图谱分析和多成分同时定量的双鱼颗粒质量评价研究

Quality assessment of Shuangyu Granules based on simultaneous determination by HPLC fingerprint and multi-components

目的 建立双鱼颗粒（SG）指纹图谱,并进行多成分定量分析,为评价SG提供依据。方法 采用Kromasil C18（250mm×4.6 mm,3.5μm）色谱柱,以乙腈-0.05%三氟乙酸水溶液梯度洗脱,体积流量0.8 m L/min,柱温30℃,检测波长为230、327 nm。采用Q-TOF/MS对指纹图谱中共有峰进行指认。结果 得到分离度、重现性均较好的SG指纹图谱,标示出17个共有峰,10批样品相似度均大于0.95;采用LC/Q-TOF/MS方法指认了14个共有峰,其中7个共有峰经对照品比对,分别为芍药苷、绿原酸、隐绿原酸、异绿原酸A、异绿原酸B、异绿原酸C和新绿原酸,并对这7个成分进行了定量分析,平均回收率在97.8%～101.8%,RSD均小于2%。结论 本方法能够快速、简便、准确地对SG指纹图谱及7个指标成分同时进行分析,可作为全面评价该制剂质量的有效方法。

Objective To establish an HPLC fingerprint chromatography and determine seven compounds of multi-components in Shuangyu Granules （SG）. Methods The Kromasil C18 （250 mm × 4.6 mm, 3.5μm） column was used with a mobile phase of acetonitrile-0.05% trifluoroacetic acid gradient elution. The flow rate was 0.8 mL/min, the column temperature was 30 , and the detection wavelengths were 230 and 327 nm. The common peaks were identified by Q-TOF/MS. Results The fingerprint chromatography included 17 mutual peaks, and the similarity was more than 0.95. Fourteen common peaks had been identified by LC-Q-TOF/MS, seven of which were unequivocally identified via comparing the retention times and mass spectra data with those of the standard compounds. Then the seven marker components were quantified. The developed quantitative method was validated in terms of accuracy （the recoveries ranged from 97.8% to 101.8% with RSDs less than 2%）. Conclusion The method is rapid, simple, and accurate and can be used for the quality control of SG.