清上蠲痛汤标准汤剂挥发油的UPLC特征图谱建立及成分分析

Establishment of UPLC characteristic chromatogram and component analysis of the volatile oil in the standard decoction of Qingshang juantong decoction

目的建立清上蠲痛汤标准汤剂挥发油的特征图谱,初步推断该方中影响临床治疗效果的主要挥发油类活性成分。方法采用水蒸气蒸馏法提取清上蠲痛汤标准汤剂中挥发油,采用《中药色谱指纹图谱相似度评价系统(2012版)》建立15批样品的超高效液相色谱(UPLC)特征图谱并进行相似度评价;采用超高效液相色谱四极杆飞行时间串联质谱(UPLC-Q-TOF/MS)法对标准汤剂挥发油类成分进行指认、鉴定;采用气质联用(GC-MS)法分析其挥发油类成分组成。结果15批清上蠲痛汤标准汤剂挥发油的UPLC特征图谱的相似度在0.949~0.997之间;共得到12个共有峰,经UPLC-Q-TOF/MS鉴定主要成分为甲基丁香酚、E-藁本内酯、E-正丁烯基苯酞等。GC-MS共鉴定出23个成分,主要为3,4,5-三甲氧基甲苯、百秋李醇、Z-藁本内酯等。结论建立了清上蠲痛汤标准汤剂挥发油的特征图谱,初步推断甲基丁香酚、藁本内酯、E-正丁烯基苯酞、百秋李醇、3,4,5-三甲氧基甲苯可能是影响清上蠲痛汤挥发油临床治疗效果的主要活性成分。

OBJECTIVE To establish the characteristic chromatogram of the volatile oil in the standard decoction of Qingshang juantong decoction,and preliminarily infer the main active components of volatile oil that affect the clinical therapeutic effect.METHODS The volatile oil in the standard decoction of Qingshang juantong decoction was extracted by steam distillation.The ultra-high performance liquid chromatography(UPLC)characteristic chromatograms of 15 batches of samples were established by the Similarity Evaluation System of TCM Chromatographic Fingerprint(2012 edition),and the similarity evaluation was carried out.The volatile oil of standard decoction was identified by UPLC coupled with quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF/MS).Then the volatile oil components were analyzed by GC-MS.RESULTS The similarities of UPLC characteristic chromatograms for volatile oil of 15 batches of Qingshang juantong decoction were between 0.949 and 0.997.A total of 12 common peaks were obtained.According to the UPLC-Q-TOF/MS,the main components were methyl eugenol,E-ligustilide,E-butylidenephthalide and so on.A total of 23 components were identified by GC-MS,which were mainly 3,4,5-trimethoxymethylbenzene,patchouli alcohol,Z-ligustilide and so on.CONCLUSIONS The characteristic chromatograms of the volatile oil in the standard decoction of Qingshang juantong decoction is established,and it is inferred that methyl eugenol,ligustilide,Ebutylidenephthalide,patchouli alcohol,3,4,5-trimethoxy-methylbenzene might be the main active components affecting the clinical therapeutic effect of the volatile oil of Qingshang juantong decoction.