GC-MS/MS法测定金牛眼药、拨云散眼药、特灵眼药中麝香酮的含量  

Determination of muscone in Jinniu eye medicine,Boyunsan eye medicine and Teling eye medicine by using GC-MS/MS

作　　者：王晓蕾 袁浩 王常顺 刘永利 WANG Xiaolei;YUAN Hao;WANG Changshun;LIU Yongli(Hebei Institute for Drug Control,Shijiazhuang,Hebei 050011,China)

机构地区：[1]河北省药品检验研究院

出　　处：《河北工业科技》2019年第5期357-361,共5页Hebei Journal of Industrial Science and Technology

基　　金：河北省科技计划项目(17272504D)

摘　　要：为了全面有效地评价眼药的内在质量,针对眼药质量标准中均未设置与人工麝香相关质控指标的现状,研究了GC-MS/MS法测定金牛眼药、拨云散眼药、特灵眼药中麝香酮含量的方法。采用HP-5MS毛细管柱(30m×0.25mm×0.25μm),分流进样,分流比为3∶1,进样量为1μL,程序升温,选择电子轰击源(EI源),多反应监测模式(MRM)进行测定,监测离子对及电压为m/z238.30>98.10(CE6),m/z209.20>95.20(CE12),m/z209.20>109.20(CE9)。结果表明,麝香酮保留时间为10.30min,线性范围为53.18~1329.6ng(r=0.9994),金牛眼药、拨云散眼药、特灵眼药的加样回收率(n=9)分别为95.2%,95.5%和95.1%,RSD值分别为1.5%,1.9%和1.2%。研究方法简便准确,重复性良好,可用于金牛眼药、拨云散眼药、特灵眼药中人工麝香含量的控制,为全面评价眼药质量提供技术支撑。In order to comprehensively and effectively evaluate the internal quality of eye drops,a GC-MS/MS method is established to determine the content of muscone in Jinniu eye medicine,Boyunsan eye medicine and Teling eye medicine in view of the current situation that no quality control index related to artificial musk is set in the quality standard of eye medicines.HP-5MS capillary column (30 m×0.25 mm×0.25 μm) is used for split injection with a split ratio of 3∶1,an injection volume of 1 μL,and programmed temperature.The electron bombardment source (EI source) and the multiple reaction monitoring mode (MRM) are selected.The monitored ions and voltage are: m/z 238.30>98.10 (CE6),m/z 209.20>95.20 (CE 12),m/z 209.20>109.20 (CE 9).The results show when the retention time of muscone is 10.30 min,the linear range is of 53.18~ 1 329.6 ng ( r =0.999 4).The recovery rate ( n =9) of Jinniu eye medicine,Boyunsan eye medicine and Teling eye medicine are 95.2%,95.5% and 95.1%,with RSD of 1.5%,1.9% and 1.2%,respectively.The method is simple,accurate and has good repeatability.It can be used to control the content of artificial musk in Jinniu eye medicine,Boyunsan eye medicine and Teling eye medicine,providing technical support for comprehensive evaluation of the quality of eye medicine.

关 键 词：中药化学 麝香酮 含量测定 GC-MS/MS法 眼药 

分 类 号：R282.5[医药卫生—中药学]