基于GC-MS同时测定蓬莪术及其醋制品挥发油中β-榄香烯、莪术醇、吉马酮、新莪术二酮的含量

Simultaneous determination of β-elemene,curcumol,germacrone and neocurdione in olatile oil of Curcuma phaeocaulis and vinegar products by GC-MS

建立一种同时测定蓬莪术及其醋制品挥发油中β-榄香烯、莪术醇、吉马酮、新莪术二酮4种主要有效成分的分析方法,为完善蓬莪术和醋制品挥发油及其制剂的质量控制提供依据,并为进一步优化蓬莪术炮制工艺及机制研究奠定基础。采用GC-MS,以正十三烷为内标物,同时对蓬莪术挥发油中4种主要有效成分进行定量分析。色谱条件为Agilent 19091S-433柱(0.25μm×250μm×30 m),进样口温度250℃,初始温度60℃,保持1 min,以5℃·min^(-1)速率升温至110℃,保持5 min,以1℃·min^(-1)速率升温至140℃,以5℃·min^(-1)速率升温至160℃,以10℃·min^(-1)速率升温至240℃,载气为氦气,流速1.0mL·min^(-1),进样量1μL。质谱条件为EI源,轰击电压70 eV;正离子模式,离子源温度200℃,以选择离子检测(SIM)定量,选择m/z 85.1,93.1,121.1,107.1,180.1分别为正十三烷、β-榄香烯、莪术醇、吉马酮、新莪术二酮的检测离子。蓬莪术挥发油中β-榄香烯、莪术醇、吉马酮、新莪术二酮全部检出,分离效果较好;在各自浓度范围内均有良好的线性关系;平均回收率在98.2%~101%。经过方法学验证,该方法可有效地对蓬莪术和醋制品挥发油及其相关制剂的质量进行控制。

This study aims to develop a method for determination of β-elemene, curcumol, germacrone and neocurdione in the volatile oil of Curcuma phaeocaulis, and to provide the basis of the quality control method for the volatile oil of C. phaeocaulis and the related preparations. Based on GC-MS, the 4 main compounds were simultaneously determined, with the internal standard n-tridecane. The Agilent 19091S-433 column （0.25 μm×250 μm×30 m） was adopted at the temperature of 250℃, the programmed temperature method （60℃ for 1min, 5℃·min^-1 to 110℃ for 5 min, 1℃·min^-1 to 140℃, 5℃·min^-1 to 160℃, 10℃·min^-1 to 240℃） was used. Helium gas was used as the carrier gas at a constant flow rat of 1 mL·min^-1, with an injection volume of 1 μL. Mass spectra were taken at 70 eV;the ion-source temperature was 200℃. The relation time and character acteristic ions for each target compound were determined by full scan mode and SIM, and m/z 85.1, 93.1, 121.1, 107.1 and 180.1 were the detection ions of n-tridecane, β-elemene, curcumol, germacrone and neocurdione. As a result, β-elemene, curcumol, germacrone and neocurdione were all detected with good separation. They were all in a good linear relationship within each concentration scope. The average recovery rates were in the range of 98.2%-101%. So, the method can be used to control the quality of the volatile of C. phaeocaulis Val. and the preparations related.