GC-MS测定香砂平胃丸中乙酸龙脑酯的含量

Determination of Bornyl Acetate in Xiangshapingwei Pills by GC-MS

目的建立GC-MS测定香砂平胃丸中乙酸龙脑酯含量的方法。方法采用DB-5MS UI毛细管柱,高纯氦气为载气,流速：1.0m L·min^-1;进样口温度：250℃,程序升温模式,起始70℃,保持2min,以20℃/min的速率升温至210℃,保持1min;质谱检测器检测,溶剂延迟3min,选择离子监测（SIM）模式,监测定量离子m/z 121、136;样品粉碎后采用无水乙醇超声提取。结果乙酸龙脑酯在0.205-8.216μg·m L^-1（r=0.0.9998）范围内线性关系良好,平均回收率为103.71%、RSD为2.57%（n=6）,最低检出限为0.0082μg·m L^-1。结论该方法简便可靠,灵敏度高,可控制香砂平胃丸的质量。

OBJECTIVE To establish a method for the determination of bornyl acetate in Xiangshapingwei Pills by GC-MS.METHODS DB-5MS UI column was used with the carries gas of Helium and the flow rate of carries gas was 1.0 mL·min ^-1;the inlet temperature was 250℃;the column temperature rose by program：the initial temperature was 70℃and maintained for 2min,and rose at 20℃/min up to 210℃ for 1min.The MSD detector was used and the time of solvent delay was 3 min;selected ion monitorine mode was used with the target quantitative ion of m /z 121 ,136.Crushed samples were extracted by anhydrous ethanol.RESULTS The linearities of bornyl acetate was fairly good and linear ranges was 0.205-8.216μg ·mL^-1 （ r=0.0.9998 ）;the average recoveries was 103.71%with RSD of 2.57%（n=6）;the limit of detection was 0.0082μg·mL^-1.CONCLUSION The method is simple,reliable and high sensitive ,it can be used for quality control of Xiangshapingwei Pills.