毛细管气相色谱法同时测定沉香化气丸中3个成分的含量

目的:建立以毛细管气相色谱同时测定沉香化气丸中乙酸龙脑酯、百秋李醇、去氢木香内酯含量的方法。方法:采用SE-30(30.0 m×0.25 mm×0.25 μm)色谱柱;以正十二烷为内标;柱温采用程序升温:起始温度120℃,保持5 min,以10℃·min^-1升温至160℃,保持5 min,再以10℃·min^-1升温至240℃,保持5 min;气化温度:260℃;检测器温度:280℃;载气为氮气,流速为3.0 mL·min^-1;进样量为1 μL,分流比为30:1。结果:在选定的条件下,乙酸龙脑酯、百秋李醇、去氢木香内酯浓度分别在0.029~1.164 mg·mL^-1(r=0.9999)、0.045~1.613 mg·mL^-1(r=0.9999)、0.037~1.339 mg·mL^-1(r=0.9995)范围内,各成分浓度与内标浓度的比值与其相应的峰面积比值呈良好的线性;平均回收率(n=9)分别为99.7%,99.5%,99.3%。结论:该方法简便准确,重复性好,可用于同时测定沉香化气丸中乙酸龙脑酯、百秋李醇、去氢木香内酯的含量。

Objective:To develop a GC method for the determination of bornyl acetate, patchouli alcohol, dehydrocostus lactone in Chenxiang Huaqi pills. Methods:The GC was performed on a SE-30 capillary column(30.0 m×0.25 mm×0.25 μm) with an FID detector, and n-dodecane was adopted as the internal standard. The temperature program of column was set as follow:the initial temperature was 120℃ and kept for 5 minutes, then increased to 160℃ at a rate of 10℃·min^-1 and maintained for 5 minutes, after that the temperature would rise to at 240℃ by 10℃·min^-1, held for another 5 minutes. The injector temperature was 260℃ and detector temperature was set at 280℃. Nitrogen was used as carrier gas at the flow rate of 3.0 mL·min^-1. The injection volume was 1 μL, and injection split ratio was 30:1. Results:Under certain chromatogram condition, the calibration curves of bornyl acetate, patchouli alcohol and dehydrocostus lactone were linear in the concentration range of 0.029-1.164 mg·mL^-1(r=0.9999), 0.045-1.613 mg·mL^-1(r=0.9999), and 0.037-1.339 mg·mL^-1(r=0.9995),respectively. The average recoveries(n=9) were 99.7%,99.5%,and 99.3%. Conclusions:The method is simple,accurate,and reproducible, which is suitable for the component determination of bornyl acetate, patchouli alcohol, dehydrocostus lactone in Chenxiang Huaqi pills.