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目的:建立同时测定消喘膏中芥子碱硫氰酸盐、延胡索乙素和细辛脂素含量的方法。方法:采用液相色谱-串联质谱联用技术。色谱柱为Waters Symmetry C18(150 mm×2.10 mm,5μm),流动相为甲醇(0.2%甲酸和2 mmol/L甲酸铵)和水(0.2%甲酸和2 mmol/L甲酸铵),梯度洗脱;质谱条件:采用电喷雾离子源正离子模式,通过多反应监测(MRM)模式同时监测复方中3种成分。结果:3种成分线性回归方程的r值均≥0.9990。平均加样回收率为71.4%~88.7%,RSD范围为7.3%~11.1%(n均为6)。结论:本法简便、快速、灵敏度高、专属性好,可用于消喘膏中芥子碱硫氰酸盐、延胡索乙素和细辛脂素的含量测定。
Objective: To establish a method for simultaneous determination of sinapine thiocyanate, tetrahydropalmatine and asarone in Ephedra extract. Methods: Liquid chromatography-tandem mass spectrometry (LC-MS / MS) was used. The chromatographic column was Waters Symmetry C18 (150 mm × 2.10 mm, 5 μm). The mobile phase consisted of methanol (0.2% formic acid and 2 mmol / L ammonium formate) and water (0.2% formic acid and 2 mmol / L ammonium formate) ; Mass spectrometry conditions: The electrospray ionization positive ion mode was used to simultaneously monitor the three components in the compound through multiple reaction monitoring (MRM) mode. Results: The r values of the linear regression equations of three components were both ≥0.9990. The average recovery rates ranged from 71.4% to 88.7% with RSD ranging from 7.3% to 11.1% (n = 6). Conclusion: The method is simple, rapid, sensitive and specific. It can be used to determine the content of sinapine thiocyanate, tetrahydropalmatine and sebacicin in XiaoChuan cream.