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目的建立银翘清热片(YQT)的HPLC指纹图谱,并采用电喷雾离子源-四极杆-飞行时间质谱(ESI-Q-TOF/MS)对其化学成分进行定性分析。方法采用Kromasil C18柱(250 mm×4.6 mm,5μm),以乙腈-0.1%磷酸水溶液梯度洗脱,体积流量为1 mL/min,柱温为25℃,检测波长为230 nm。ESI-Q-TOF/MS正、负2种离子模式扫描对其化学成分定性分析。结果建立了YQT HPLC指纹图谱,标定28个共有峰,归属到6味药材,其中7个共有峰来源于连翘,9个共有峰来源于金银花,6个共有峰来源于葛根,3个共有峰来源于牛蒡子,1个共有峰(2号)来源于连翘和升麻,另外2个共有峰分别来源于知母和升麻。11批不同批次的YQT制剂相似度均大于0.95。并采用LC-Q-TOF/MS方法鉴定了42个化学成分,其中16个采用对照品比对鉴定,分别为葛根素、大豆苷、大豆苷元、新绿原酸、绿原酸、隐绿原酸、异绿原酸A、异绿原酸B、异绿原酸C、断氧化马钱苷、芦丁、连翘苷、连翘酯苷A、牛蒡苷、芒果苷、知母皂苷B II。结论完善了YQT的质量标准体系,可为同类型的其他复方制剂的物质基础研究和质量控制提供参考。
OBJECTIVE To establish the HPLC fingerprint of YQT and analyze its chemical composition by electrospray ionization-quadrupole-time of flight mass spectrometry (ESI-Q-TOF / MS). The method was performed on a Kromasil C18 column (250 mm × 4.6 mm, 5 μm) with a gradient of acetonitrile-0.1% phosphoric acid. The volume flow rate was 1 mL / min. The column temperature was 25 ℃ and the detection wavelength was 230 nm. ESI-Q-TOF / MS positive and negative ion mode scanning of two qualitative analysis of its chemical composition. Results YQT HPLC fingerprints were established, 28 common peaks were assigned to 6 herbs, of which 7 common peaks originated from Forsythia, 9 common peaks from honeysuckle, 6 common peaks from Pueraria, 3 common peaks Originated from Arctium lappa, one common peak (No.2) originated from Forsythia and Cimicifuga, and the other two common peaks originated from Anemarrhena and Cimicifuga respectively. The similarity of 11 batches of YQT preparations were all greater than 0.95. Forty-two chemical constituents were identified by LC-Q-TOF / MS method, of which 16 were identified by the comparison of reference materials, namely puerarin, daidzin, daidzein, neogenin, chlorogenic acid, Acid, Isocrochloric Acid A, Isocrochloric Acid B, Isocrochloric Acid C, Digoxigenin, Rutin, Forsythin, Forsythoside A, Arctiin, Mangiferin, Tartarini B II . Conclusion The quality standard system of YQT has been improved, which can provide references for the material basic research and quality control of the same type of other compound preparations.