目的 建立柴胡舒肝丸挥发性成分的气相色谱-质谱(GC-MS)指纹图谱.方法 采用超声提取法提取柴胡舒肝丸中的挥发性成分;采用GC-MS法进行分离、鉴定,色谱柱为Shimadzu HP-5MS毛细管柱(30 m×0.25 mm,0.25μm),载气为氦气(纯度≥99.999%),流速为 1.0 mL/min,进样口温度为 250℃,进样量为 1μL,分流比为 20∶1,电子轰击离子源,轰击能量为 70 eV,离子源和传输线温度分别为 230,250℃,溶剂延迟时间为 4 min,数据扫描模式为全扫描,质荷比(m/z)为 55~550.采用中药色谱指纹图谱相似度评价系统(2004A)软件进行共有峰指认,结合美国国家标准与技术局(NIST)谱库检索及相关文献确定化合物名称,指明峰归属;采用面积归一化法计算各成分的含量,并进行聚类分析.结果 14 批样品有 47 个共有峰,鉴定化学成分 37 种(占总峰面积的 96%以上),主要化学成分包括厚朴酚(12.25%)、薄荷酮(11.69%)、β-谷甾醇(8.66%)、十六烷酸(7.28%)等.14 批样品共聚为两类,其中编号为S5 和S6 的样品聚为Ⅰ类,编号为S1-S4 和S7-S14 的样品聚为Ⅱ类.结论 所建立的GC-MS指纹图谱稳定、可靠,可用于柴胡舒肝丸挥发性成分的研究及整体质量控制.
Objective To establish a gas chromatography-mass spectrometry(GC-MS)fingerprint of volatile components in Chaihu Shugan Pills.Methods Ultrasound extraction was used to extract the volatile components in Chaihu Shugan Pills,and GC-MS method was used for separation and identification,the chromatographic column was Shimadzu HP-5MS capillary column(30 m×0.25 mm,0.25 μm),the carrier gas was helium(purity≥99.999%),the flow rate was 1.0 mL/min,the temperature of injection port was 250℃,the injection volume was 1 μL,the diversion ratio was 20∶1.Electron bombardment ion source was adopted with bombardment energy of 70 eV,the temperature of ion source and transmission line was set at 230℃and 250℃,the solvent delay time was 4 min,data scanning mode was adopted for full scan,the charge to mass ratio(m/z)was 55-550.The Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine(Version 2004A)software was used to identify common peaks.According to the standard mass spectrometry database of the National Institute of Standards and Technology(NIST)and literature search,the names of components were determined,and the peak attribution was identified.The content of each component was calculated by the area normalization method,and cluster analysis was performed.Results There were 47 common peaks in 14 batches of samples,and 37 chemical components were identified(accounting for more than 96%of the total peak area).The main chemical components included magnolol(12.25%),menthone(11.69%),β-sitosterol(8.66%),palmiticacid(7.28%),etc.Fourteen batches of samples were clustered into two categories,with samples numbered S5 and S6 clustered into category Ⅰ,and samples numbered S1-S4 and S7-S14 clustered into category Ⅱ.Conclusion The established GC-MS fingerprint is stable and reliable,which can be used for the study of volatile components and overall quality control of Chaihu Shugan Pills.