GC-MS法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  

Simultaneous determination of muscone,β-asarone,patchoulic alcohol, borneol,menthol in compound Shexiang injection by GC-MS

作　　者：彭敏[1] 邓楠[1] 刘文[1] 戴迎春[1] 

机构地区：[1]湖南省人民医院药学部临床药学办,长沙410002

出　　处：《药物分析杂志》2014年第5期855-858,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：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×0.25μm×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1μL,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-1to 190 ℃ for 1. 5 min,then 40 ℃ · min-1to 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.

关 键 词：复方麝香注射液 麝香酮 Β-细辛醚 百秋李醇 龙脑 薄荷脑 有效成分 质量控制 气相色谱-质谱联用 

分 类 号：R917[医药卫生—药物分析学]