达立通颗粒的HPLC指纹图谱研究及其LC-MS化学成分分析

HPLC Fingerprint and LC-MS Chemical Constituents Analysis of Dalitong Granules

目的:建立达立通颗粒的HPLC指纹图谱,并对达立通颗粒的化学成分进行鉴定。方法:采用Hypersil ODS-BP色谱柱(250 mm×4.6 mm,5μm);流动相为乙腈-0.05%乙酸溶液,梯度洗脱;检测波长为323 nm;柱温为30℃;流速为1.0 mL/min;进样量为10μL。采用"中药色谱指纹图谱相似度评价系统(2012版)"进行相似度分析。采用Triple TOF 5600+型检测器,运用ESI源分别在正、负模式下对达立通颗粒进行分析检测,并对达立通颗粒的12味原药材进行成分归属。结果:建立了达立通颗粒的HPLC指纹图谱,标定了16个共有峰,指证了其中4个共有峰分别为绿原酸、咖啡酸、芦丁和橙皮苷。10批达立通颗粒HPLC指纹图谱的相似度均大于0.990,通过LC-MS技术对达立通颗粒中的35个化学成分进行了鉴定。结论:该方法简单、快捷、稳定,可用于达立通颗粒的质量控制。

Objective:To establish the HPLC fingerprint of Dalitong granules,and to characterize the chemical constituents by LC-MS.Methods:The HPLC method was established by using Hypersil ODS-BP chromatographic column(250 mm×4.6 mm,5μm)with acetonitrile-0.05%acetic acid aqueous solution as mobile phase in a gradient elution.The detection wavelength was 323 nm,the column temperature was 30℃,the flow rate was 1.0 mL/min,the injection volue was 10μL.The"Similarity evaluation system for chromatographic fingerprint of TCM(Version 2012)"software was employed to carry out the similarity analysis.The Triple TOF 5600+detector and the ESI source in positive and negative modes were used to analysis the Dalitong granules.The twelve original medicinal materials of Dalitong granules were classified.Results:The HPLC fingerprint of Dalitong granules was established,sixteen common peaks were obtained,four common peaks were identified as chlorogenic acid,caffeic acid,rutin and hesperidin.The HPLC fingerprint similarity of ten batches of Dalitong granules was over 0.990.Thirty-five chemical constituents of Dalitong granules were identified by LC-MS.Conclusion:This method is simple,fast and stable,and can be used for the quality control of Dalitong granules.