加味西黄软胶囊中胆酸、麝香酮的含量测定

Determination of cholic acid and muscone in Jawei Xihuang Soft Capsule

目的:建立反相高效液相色谱-蒸发光散射检测法(HPLC-ELSD)测定加味西黄软胶囊(牛黄、麝香、蟾酥、乳香、没药)中胆酸的含量;建立气相色谱法测定加味西黄软胶囊中麝香酮的含量。方法:胆酸采用十八烷基键合硅胶色谱柱(Kromasil C18,5μm,4.6mm×250mm),流动相为甲醇-0.1%冰醋酸(73∶27),流速:1.0mL/min;ELSD检测器参数:蒸发温度40℃,载气(N2)压力200kPa。麝香酮的含量测定以正十八烷为内标物,采用DB-1型毛细管色谱柱(30m×0.32mm×0.25μm);FID检测器;程序升温。结果:胆酸在45.2～904ng范围内呈良好的线性关系,平均回收率为99.06%,RSD为1.56%。麝香酮在0.05～0.5mg/mL范围内与峰面积比值的线性关系良好,平均回收率为99.40%,RSD为0.95%。结论:本方法简便、准确,可用于该制剂的质量评价。

AIM：To develop a method for determining cholic acid by HPLC-ELSD and GC was applied to determing muscone;in Jawei Xihuang Soft Capsule（Calculus Bovis,Moschus,Venenum Bufonis,Olibanum,Myrrha）.METHODS：A C18 column（Kromasil C18,5 μm,4.6 mm×250 mm）was used as stationary phase,the mobile phase was methanol-0.01% glacial acetic acid（73：27） at a flow rate of 1.0 mL/min.The parameters of ELSD were set as follows：evaporation temperature was 40 ℃,carrier gas（N2） pressure was 200 kPa.The GC system consisted of DB-1 capillary column（30 m×0.32 mm×0.25 μm） and FID as the detector.The programmed temperature-GC and internal standard method were employed to determine the content of muscone.RESULTS：The linear ranges of cholic acid and muscone were in the range of 45.2 ng-904 ng and 0.05 mg/mL—0.5 mg/mL respectively.The average recoveries were 99.06% and 99.40% with RSD of 1.56% and 0.95% respectively.CONCLUSION：The method is convenient and accurate,and it can be used for the quality evaluation of Jawei Xihuang Soft Capsule.