逍遥散的GC-MS特征图谱研究

目的: 应用气相色谱-质谱(GC-MS)法建立逍遥散挥发性成分的特征图谱。 方法: 采用5HP-MS色谱柱(0.25 mm×30 m,0.25 μm),He为载气,流速为1.0 mL·min^-1,进样量为1 μL,分流比为1: 30。电子轰击(EI)离子源,辅助线温度为280 ℃,离子源温度为230 ℃,四极杆温度为150 ℃;质量扫描范围m/z 30~600;Chemstation和Nist 05a谱库检索,对10批逍遥散样品进行了分析。 结果: 通过分析10个批次的逍遥散,确定了29个共有色谱峰,鉴定了其中28个。采用中药色谱指纹图谱相似度评价系统软件(2004A版)对其特征性图谱分析的结果显示,10批逍遥散样品相似度均在0.90以上。 结论: 逍遥散的GC-MS特征图谱特征性及专属性强,该特征图谱为逍遥散挥发性成分质量控制提供了重要依据。

Objective: To establish the gas chromatography-mass spectrometry(GC-MS) characteristic chromatograms for the quality control of Xiaoyao powder. Methods: The GC-MS analysis was performed on a 5HP-MS column(0.25 mm×30 m,0.25 μm) with helium as the carrier gas. The flow rate was set at 1.0 mL·min^-1, and the injection volume was 1 μL. Electron impact(EI) was used as the electron source and the spectra were recorded in the m/z range of 30-600. The temperatures of auxiliary line, icon source and quadrupole were 280 ℃, 230 ℃ and 150 ℃. GC-MS characteristic chromatograms of 10 batches of Xiaoyao powder samples were analyzed by this GC-MS method and were evaluated by Chemstation and Nist 05a system. Results: Among 10 batches of Xiaoyao powder, 29 common peaks were defined,of which 28 peaks were identified. Similarity Evaluation System for Chromatographic Fingerprint of TCM (2004A) was used to analyze the 10 batches of Xiaoyao powder, which showed the similarity of fingerprints was more than 0.90. Conclusion: The developed characteristic chromatograms method is reliable and accurate, which can be used for the quality control of volatile components in Xiaoyao powder.