GC-MS法同时测定蛇床子中7种香豆素类活性成分

Simultaneous quantification of 7 coumarins in common cnidium fruit by GC-MS

建立了同时测定蛇床子中7种香豆素类活性成分的GC-MS分析方法。采用DB-1毛细管柱(30 m×0.25 mm×0.25μm),柱温采用程序升温,接口温度280℃,离子源温度250℃,四极杆温度150℃,采用电子轰击离子化(EI源)电离方式,电子能量70 e V,选择离子检测模式(SIM),扫描范围为50~350 amu。考察了方法的灵敏度、线性范围、回收率、日内和日间精密度。在本方法条件下,7种香豆素类活性成分的线性关系良好(r^2≥0.998 6),检测限和定量限分别为1.06~10.11 ng·m L^(-1)和3.21~29.88 ng·mL^(-1)。日内(n=6)和日间(n=3)精密度分别为0.7%~2.5%和1.2%~3.3%。平均回收率范围为92.38%~100.50%。本方法简便、快速、灵敏度高、专属性好,可为蛇床子药材的质量控制提供参考依据。

A GC-MS-SIM method was developed for the simultaneous determination of the 7 coumarins in common cnidium fruit. The 7 bioactive constituents were separated on DB-1 capillary column（30 m × 0.25 mm, 0.25 μm） using temperature programming. The interface temperature was set at 280 ℃; Ion source temperature： 250 ℃; Quadrupole temperature： 150 ℃; EI mode： 70 e V; The mass spectrometer detector was in SIM mode; Scan range： 50-350 amu. All the 7 marker substances showed good linearity（r2 〉0.998 6） in the test ranges. The LODs and LOQs for the compounds ranged from 1.06 to 10.11 ng·mL^（-1） and from 3.21 to 29.88 ng·m L^（-1）, respectively. The overall intra-day（n = 6） and inter-day（n = 3） RSDs were 0.7%-2.5% and 1.2%-3.3%, respectively. The overall recoveries were between 92.38% and 100.50% for all compounds. This method was simple, rapid, sensitive, with good specificity, and it can provide a reference for the quality control of common cnidium fruit.