加速溶剂萃取/气相色谱-三重四极杆质谱测定石菖蒲中的α-细辛脑和β-细辛脑

目的: 建立加速溶剂萃取/气相色谱-三重四极杆质谱(GC-MS/MS)测定石菖蒲中的细辛脑含量方法。 方法: 为了取得最佳的萃取效果,优化萃取溶剂、温度、静态萃取时间和次数等加速溶剂萃取条件。萃取液稀释后直接通过GC-MS/MS分析,多反应监测模式检测细辛脑,以保留时间和特征离子对(母离子(m/z)为208.2和2个子离子(m/z)为192.8和164.8)信息比较进行定性定量分析,外标法定量。 结果: 选择甲醇为萃取试剂,120℃静态萃取5.0 min共2次,则萃取效率最佳。细辛脑在DB-1701毛细管柱上实现基线分离,α-细辛脑和β-细辛脑。结论: 本法提取效率高,定量准确,定性可靠,可用于石菖蒲中细辛脑的含量测定及质量评价。

Objective: To develop a sensitive and reliable method for the analysis of asarone in Acorus tatarinowii Schott using accelerated solvent extraction(ASE) and gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). Methods: The ASE parameters (extraction solvent and temperature, static time and cycle) were optimized in order to maximize the extraction efficiency. The ASE extract was diluted with methanol. The asarone was determined by GC-MS/MS in multiple reactions monitoring (MRM) modes. The qualitative and quantitative analysis was performed base on the retention time and the characteristic ion-pairs consisting of one precursor ion (m/z) of 208.2 and two product ions (m/z) of 192.8 and 164.8. The contents of asarone were quantified by external standard method. Results: Optimal results were achieved by using methanol as extraction solvent at a temperature of 120℃, and applying two cycle of extraction with a static time of 5.0 min. A good GC separation was achieved using a DB-1701 capillary column. The detection limits of α-asarone and β-asarone were 0.2 μg·L^-1 and 0.5 μg·L^-1, respectively. Conclusion: The method is highly efficient in extraction, accurate quantitative and reliable qualitative, which can be used for determination of asarone in Acorus tatarinowii Schott.