目的：建立一种同时测定复方麝香注射液中麝香酮、β-细辛醚、百秋李醇、龙脑、薄荷脑5个成分的分析方法，为建立复方麝香注射液的质量控制方法的提供依据。方法：采用气质联用法进行测定。色谱条件：Agilent HP-5MS毛细管柱（30 m×0.25 μm×0.25 mm），进样口温度280 ℃，柱温采取程序升温（初始温度100 ℃，保持2 min，以5 ℃·min-1速率升温至190 ℃，保持1.5 min，以40 ℃·min-1速率升温至250 ℃），载气为高纯氦气，流速为1 mL·min-1，进样量为1 μL，分流比5：1；质谱条件：EI源，轰击电压70 eV，离子源温度230 ℃，四极杆温度150 ℃，辅助接口温度280 ℃，采用全扫描模式获得混合对照品溶液的总离子流色谱图，确定各目标化合物的保留时间和特征离子，再进行选择离子检测（SIM）定量，选择m/z 238、208、222、138、154分别为麝香酮、β-细辛醚、百秋李醇、龙脑和薄荷脑的检测离子。通过外标法同时对复方麝香注射液中5个主要有效成分进行定量分析。结果：复方麝香注射液中麝香酮，β-细辛醚，百秋李醇，龙脑，薄荷脑在23 min内全部检出，且分离效果较好；在各自的浓度范围内均有良好的线性关系（r均为0.99以上）；平均回收率在98.8%~102.0%范围内。结论：该方法经过方法学验证，可有效地对复方麝香注射液的质量进行控制。
Objective: To develop a method for determination of muscone,β-asarone,patchoulic alcohol,borneol,menthol in compound Shexiang injection,and to provide the basis for establishing the quality control method for compound Shexiang injection. Methods: GC-MS method was adopted.Chromatographic conditions were as follows: the Agilent HP-5MS column (30 m×0.25 μm×0.25 mm) was adopted at the injector temperature of 280 ℃,the programmed temperature method (100 ℃ for 2 min,5 ℃·min-1 to 190 ℃ for 1.5 min,then 40 ℃·min-1 to 250 ℃) was used.Helium gas was used as the carrier gas at a constant flow rate of 1 mL·min-1,with an injection volume of 1 μL (split ratio of 5:1).Mass spectra were taken at 70 eV;the ion-source temperature was 280 ℃,the quadrupole temperature 150 ℃,the auxiliary interface temperature 280 ℃.The retention time and characteristic ions for each target compound were determined by full scan mode and SIM,and m/z 238,208,222,138,154 were the detection ions of muscone,β-asarone,patchoulic alcohol,borneol,menthol.The five main effective constituents of compound Shexiang injection were analyzed with external standard method via GC-MS. Results: Muscone,β-asarone,patchoulic alcohol,borneol and menthol in compund Shexiang injection were all detected in 23 min with good separation.Muscone,β-asarone,patchouli alcohol,borneol and menthol were in a good linear relationship within each concentration scope (r≥0.99).The average recovery rates were in the range of 98.8%-102.0%. Conclusion: The method was validated,and can be used to control the quality of compound Shexiang injection.
