气相色谱法测定抗感至宝合剂中百秋李醇的含量

Determination of Patchouli Alcohol in Kangganzhibao Mixture by GC

目的:建立毛细管气相色谱测定抗感至宝合剂中百秋李醇含量的方法,制定并提高抗感至宝合剂质量标准。方法:样品经石油醚(30～60)℃萃取处理后进行含量测定。色谱条件:HP-5毛细管柱(0.25μm×0.25 mm×30 m);FID检测器,1 177进样口初始温度180℃,保持10 min,以每分钟5℃的速率升温至230℃,保持3 min;进样口温度280℃,检测器温度280℃,分流比37∶1,流速1 mL.min-1,进样量1μL。以正十八烷为内标,理论板数按百秋李醇峰计算不低于50 000。结果:百秋李醇进样量在0.012～0.072μg线性关系良好Y=294X+12.8,(r=0.999 6),平均加样回收率为98.45%,RSD 1.09%。结论:该方法稳定、结果可靠、重复性好,可作为抗感至宝合剂质量控制标准之一。

Objective： To establish a method for the determination of patchouli alcohol in Kangganzhibao Mixture by capillary gas chromatography,and develop and improve the quality standards of this mixture.Method： Samples were pretreated with petroleum ether（30-60 ℃）.Chromatographic condition was as follows： HP-5 capillary column（0.25 mm × 0.25 μm × 30 m）,FID detector and 1 177 injector;the column temperature was controlled by programming： the initial temperature was set at 180 ℃ for 10 min,and then rose up（5 ℃.min-1） to 230 ℃ for 3 min;the detector and injector temperature were set at 280 ℃;split ratio was 37∶ 1;the flow rate of nitrogen was 1 mL.min-1 and the injection volume was 1 μL;internal standard was n-octadecane;and the number of theoretical plates was not less than 50 000（calculated by patchouli alcohol）.Result： Patchouli alcohol was linear in the range of 0.012-0.072 μg（Y = 294X ＋ 12.8）（r = 0.999 6）.The average recovery was 98.45% with RSD 1.09%（n = 6）.Conclusion： The method is stable and reliable with good repetition,which can be used as one of the quality control methods for Kangganzhibao Mixture.