华佗救心丸GC-MS特征图谱及3个成分的含量测定

GC-MS characteristic chromatogram and assay of three components for Huatuo Jiuxin pills

目的:利用气相色谱-质谱(gas chromatography-mass spectrometry,GC-MS)联用技术,建立华佗救心丸GC-MS特征图谱,同时测定龙脑、异龙脑和麝香酮3个成分的含量。方法:采用VF-WAXms毛细管色谱柱(0.25 mm×30 m,0.25μm),柱温为程序升温(140℃,停留2 min,然后以35℃·min^(-1)线性升温至230℃,停留5 min),进样口温度:210℃,检测器温度250℃;离子源为电子轰击源(electrospray ion source,EI),离子源温度为230℃,MS四极杆温度为150℃,发射电流为34.6μA,发射能量为70.0 eV,质谱监测模式为全扫描(SCAN),溶剂延迟为3 min。应用2012版中药色谱指纹图谱相似度评价软件对12批华佗救心丸进行相似度分析,同时对龙脑、异龙脑和麝香酮3个成分含量进行测定。结果:建立了华佗救心丸的GC-MS指纹图谱,12批华佗救心丸的色谱图与特征图谱的相似度均在0.999以上,标定共有峰8个,并指认了其中3个共有峰,分别为异龙脑、龙脑和麝香酮。12批样品中龙脑、异龙脑和麝香酮的含量范围分别为每丸0.8757~1.5250 g、0.7304~1.1405 g、0.0971~0.1120 g。结论:所建立的GC-MS特征图谱结合3个成分的含量测定,能较全面地反映华佗救心丸中挥发性化学成分质量,该方法简便可行,准确稳定,重复性和专属性好,可对华佗救心丸质量控制提供参考。

Objective:To establish a GC-MS characteristic chromatogram of Huatuo Jiuxin pills and to develop simultaneous determination method of borneol,isborneol and muscone in the sample.Methods:GC-MS analysiswas performed on a VF-WAXms column(0.25 mm×30 m,0.25μm).The column temperature was programmed to start at 140℃maintaining for 2 min,and rose to 230℃at a rate of 35℃·min^(-1),maintaining for 5 min.The inlet temperature was 210℃and the detector temperature was 250℃.The ion source was electrospray ion source,with the ion source of 300℃,MS quadrupole temperature of 150℃,the emission current of 34.6μA,the ionization energy of 70 eV and the solvent delay of 3 min,quantized by the full scan method.Traditional Chinese medicine chromatographic fingerprint similarity evaluation software(2012 version)was used for similarity analysis in 12 batches of Huatuo Jiuxin pills,and the contents of borneol,isoborneol and muscone in 12 batches of samples were determined at the same time.Results:The GC-MS characteristic chromatogram of Huatuo Jiuxin pills was established,and the similarities between the characteristic chromatogram and chromatograms of 12 batches of Huatuo Jiuxin pills were above 0.999.There were altogether 8 common peaks,and 3 of them were identified as isoborneol,borneol andmuscone,respectively.The contents of borneol,isborneol and muscone in 12 batches of samples were in the range of 0.8757-1.5250,0.7304-1.1405,0.0971-0.1120 g per pill,respectively.Conclusion:The combination of the GC-MS characteristic chromatogram and content determination of three components can reflect inherent quality of volatile chemical components in Huatuo Jiuxin pills.The method is simple,feasible,accurate,stable,repeatable and specific,and can provide a reference for the quality control of Huatuo Jiuxin pills.