两种方法测定川芎油中藁本内酯、洋川芎内酯A和正丁基苯酞的含量

Simultaneous Determination of Ligustilide,Senkyunolide A And N-Butylphthalide in the Essential Oil of Chuanxiong Rhizoma by GC-MS and HPLC

目的:建立同时测定川芎油中藁本内酯、洋川芎内酯A和正丁基苯酞含量的方法,比较两种方法分析结果的差异。方法:采用超临界CO2萃取法和水蒸气蒸馏法提取川芎油,分别采用气相色谱质谱联用(GC-MS)内标法和高效液相色谱(HPLC)外标法测定,并进行方法学考察。结果:SFE-CO2萃取法和水蒸气蒸馏法的出油率分别为10.49%,1.54%,以每克药材中提取得到的藁本内酯、洋川芎内酯A和正丁基苯酞的量计算,SFE-CO2萃取法分别可得19.676,15.56,0.957 4 mg,水蒸气蒸馏法提取可得2.16,1.56,0.11 mg。GC-MS法测定结果较HPLC法低1%～4%,平均精密度高10%、检测限低10倍。结论:GC-MS内标法精密度、灵敏度都较好,对川芎油的含量的分析较为准确;HPLC法是一种相对方便、经济的方法。

Objective： To establish the simultaneous determination method for ligustilide, senkyunolide A and n-butylphthalide in the essential oil of Chuanxiong Rhizoma, and to compare the results of HPLC and GC-MS method. Method： The oil was obtained through supercritical CO2 extraction and steam distillation, and the contents of the above three compounds were determined by gas chromatography mass spectrometry （GC-MS） with internal standard method and high performance liquid chromatography （HPLC） with external standard method respectively and methodology was also inspected. Result： The oil yields were 10.49% and 1.54% respectively. The contents of the three compounds were 19.676, 15.56, 0. 957 4 mg per gram crude drug in SFE-CO2 extraction and 2. 16, 1.56 and 0. 11 mg in volatile oil which measured by GC-MS was 1%-4% less than the value which obtained by HPLC. Compared with the result by HPLC, GC-MS is more scientific with 10% higher precision and tenfold detection limit. Conclusion： In the determination of components in the essential oil of Chuanxiong Rhizoma, GC- MS internal standard method is a more accurate and sensitive method whereas HPLC is a relatively convenient and economical method.