回医香药核心方挥发性成分的分析鉴定

Identification of Chemical Constituents in Volatile from He Xin Hui Formula by GC-MS

目的分别采用水蒸气蒸馏法（SD）和超临界CO2萃取法（SFE）提取回药核心方中挥发油和小极性成分,利用气质联用法鉴定分析各成分,比较不同提取方法所得成分种类的差异。方法 Shimadzu QP2010 plus GC-MS条件：Rxi-5Sil MS（30 m×0.25 mm×0.25μm）石英毛细管柱,起始温度50℃,保留1 min,以10℃·min-1升温至120℃维持3 min,以3℃·min-1升温至200℃维持3 min,以5℃·min-1升温至290℃维持10min至完成分析;载气为氦气,柱流量1.0 ml·min-1,分流比25∶1,进样口温度250℃,EI电离源70 e V,离子源温度230℃,扫描范围m/z 35~500。结果 SD法提取挥发油得率为0.85%,共分离鉴定出40个化合物,占挥发油总质量的97.88%;SFE法提取挥发油得率为5.82%,共分离鉴定出54个化合物,占成分总质量的77.85%;结论采用SD法和SFE法提取得到的回药香药核心方的小极性成分在种类上有很大差异,GC-MS可用于鉴定和测定香药小极性成分,为下一步阐明回医香药的活性物质基础提供了实验数据。

Objective The volatile components of the Hui formula＂He Xin＂were extracted by steam distillation extraction（ SD）and supercritical CO2 fluid extraction,respectively; and the structures were analyzed and identified by GC- MS. Methods The mass spectrometric conditions were set as follows： Shimadzu QP2010 plus GC- MS,Rxi- 5Sil MS quartz capillary column（ 30 m× 0. 25 mm × 0. 25 μm）,the starting temperature 50℃,maintained 1 min,heated to 120℃ with 10℃ ·min- 1,maintained 3min,then heated to 200℃ with 3℃ ·min- 1,maintained 3 min,contincied heated to 290℃ with 5℃ ·min- 1,maintained until completion of analysis; helium as the carrier gas,column flow rate 1. 0 m L min- 1,split ration 25： 1,inlet temperature 250℃,EI ionization source 70 e V,ion source temperature 230℃,scan range of m / z 35 ~ 500. Results Yield of volatile oil were 0. 85%and 5. 81% extracted by SD and SFE methods,respectively; and for SD method,40 kinds of compounds were identified,accounted for 97. 88% of total mass of volatile oil; for SFE method,54 kinds of constituents were identified,accounted for 77. 85% of total mass of volatile oil. Conclusion The type of constituents contained in the volatile oil extracted by SD and SFE methods were totally different,and GC- MS could be used to identify the structures and relative content of volatile components,the results of this study could provide experimental basis for development and utilization of Hui medicine.