气相色谱-质谱联用法测定蛇床子超临界二氧化碳流体提取物中蛇床子素含量

Quantitative Determination of Osthole in Supercritical CO_2 Fluid Extracts of Cnidium monnieri by Gas Chromatography-Mass Spectrometry

目的 建立气相色谱-质谱联用法测定蛇床子超临界二氧化碳（C02）流体提取物中蛇床子素的含量.方法 样品采用C02超临界流体萃取,萃取液用乙酸乙酯溶解,选择监测离子法测定蛇床子素的含量.色谱条件：DB-5 MS（30 m×0.32 mm,0.25 μm）石英毛细管色谱柱;柱流速2.0 mL·min^-1,柱温60℃保持2 min,以10℃·min^-1到280℃,保持6 min;进样口和接口温度为280 ℃.结果 蛇床子素在5～1 000μg·mL^-1线性关系良好,r=0.999 1,平均回收率为98.97％,检测限1.0 ng·mL^-1.结论 该方法稳定可靠,适用于蛇床子药材的质量控制.

Objective To establish a method for content determination of osthole from Cnidium monnieri in supercritical fluid CO2（SFE-CO2） extract by gas chromatography-mass spectrometry （GC-MS）. Methods The sample was extracted from Cnidium monnieri by SFE-CO2 and solved by acetic ether. The content of ostholei determined by GC-MS with selected ion monitor（GC-MS/SIM）. Separation was performed on DB-5MS capillary column （30 m×0.32 mm,0.25 μm） at the flow rate of 2.0 mL · min^-1. The column temperature was started at 60℃ for 2 min, then increased to 280 ℃ at 10 ℃· min^-1 and maintained at 280 ℃ for 6 rain. The temperature of both interface and inlet was kept at 280 ℃. Results The linear range of osthole was within 5-1 000 μg · mL^-1 （ r = 0. 999 1 ）. The mean extraction recovery was 98.97% and limit of detection was 1.0 ng · mL^-1. Conclusion The method is reliable and stable,which can be applied to quality control of Cndium monnieri.