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

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；HPLG法是一种相对方便、经济的方法.

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

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.