逍遥散的GC-MS特征图谱研究  

GC-MS characteristic chromatograms of Xiaoyao powder

作　　者：刘海洋[1] 王盈盈[1] 于茜[1] 李建民[1] 张宁[1] 耿放[2] 

机构地区：[1]黑龙江中医药大学,哈尔滨150040 [2]哈尔滨师范大学,哈尔滨150025

出　　处：《药物分析杂志》2013年第9期1507-1511,1517,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金青年科学基金项目(81102769);黑龙江省自然科学基金面上项目(D201172);哈尔滨市科技创新人才专项资金项目(2011RFQ XS 076);教育部“春晖计划”合作科研项目(Z2010023)

摘　　要：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,0.25μm),He为载气,流速为1.0 mL·min-1,进样量为1μL,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 chromato- grams 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 Chro- matographic 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.

关 键 词：逍遥散 气相色谱-质谱 中成药特征图谱 柴胡 当归 白术 炮姜 薄荷 

分 类 号：R917[医药卫生—药物分析学]