气相色谱-串联质谱法同时测定柴胡舒肝丸10种挥发性成分

Simultaneous determination of ten volatile components in Chaihu Shugan Pills by gas chromatography-mass spectrometry

建立气相色谱-串联质谱法测定柴胡舒肝丸挥发性成分藁本内酯、α-香附酮、十六烷酸、去氢木香内酯、人参炔醇、厚朴酚、和厚朴酚、大黄酚、大黄素甲醚、β-谷甾醇含量的方法。称取5 g柴胡舒肝丸样品,以乙酸乙酯为提取溶剂,样品浸泡30 min,冰水浴超声提取10 min,以气相色谱-串联质谱法对10种挥发性成分定性,内标法定量。10种挥发性成分在对应质量浓度范围内与色谱峰面积线性关系良好,相关系数(r)均大于0.995,样品加标回收率为93.4%~102.8%,测定结果的相对标准偏差为1.2%~5.1%(n=6)。该方法重复性高、稳定性和精密度良好、专属性强、操作简便,适用于柴胡舒肝丸多组分的质量控制。

A gas chromatography-mass spectrometry method was established for simultaneous determination of 10 volatile components in Chaihu Shugan Pills,ligustilide,α-cyperone,hexadecanoic acid,dehydrocostus lactone,panaxynol,magnolol,honokiol,chrysophanol,physcion andβ-sitosterol.5 g Chaihu Shugan Pills sample was completely soaked for 30 min in ethyl acetate,and performed ultrasonic extraction in an ice water bath for 10 minutes.10 components were performed by gas chromatography-mass spectrometry and quantified by internal standard method.The linear relationship between the contents of citrinin standards concentration and chromatographic peak area was good in corresponding concentrations with a linear correlation coefficient not less than 0.995.The average recoveries of ten components was 93.4%-102.8%,and relative standard deviation 1.2%-5.1%(n=6).The method has good repeatability,stability and precision are satisfying,specific and simple,which is suitable for multi-component quality control analysis of Chaihu Shugan Pills.