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作 者:李凤丽[1,2] 高文远[3] 李进[1] 陈涛[1] 王进博[1]
机构地区:[1]天津中医药大学第一附属医院,天津300193 [2]天津中医药大学,天津300193 [3]天津大学,天津300193
出 处:《中国实验方剂学杂志》2014年第14期65-68,共4页Chinese Journal of Experimental Traditional Medical Formulae
基 金:国家"重大新药创制"科技重大专项(2010ZX09102-201)
摘 要:目的:建立并优化暑热宁口服液中百秋李醇、广藿香酮、麝香草酚、香荆芥酚的毛细管气相色谱法测定条件。方法:HP-5弹性石英毛细管柱(0.25μm×0.32mm×30m),进样口温度220℃,FID检测器温度220℃,程序升温,起始温度110℃,保持10min,以25℃程序升温至230℃,保持9.2min,分流比10:1,进样量1μL。结果:百秋李醇、广藿香酮、麝香草酚、香荆芥酚在1.109~0.1109,0.504~0.0504,0.987~0.0987,0.605~0.0605g·L^-1与峰面积线性关系良好,线性关系为Y百秋李醇=1653.05X-1.46(r=0.9998),Y广藿香酮=1207.45X-16.10(r=0.9997),Y麝香草酚=1691.68X-18.06(r=0.9995),Y香荆芥酚=1547.18X+5.55(r=0.9996),加样回收率(n:9)为99.9%~103.7%,98.4%~104.4%,96.5%~101.4%,97.2%~102.6%,RSD分别为1.9%,2.3%,2.5%,2.2%。结论:优化后的测定方法分离度较好,阴性无干扰,操作简便,结果稳定可行。Objective: Optimization and to establish the heat better oral liquid from best autumn lee alcohol, ketone of patchouli, thymol, sweet fineleaf schizonepeta.herb phenol of capillary gas chromatography determination conditions. Method: The chromatographic column- HP-5 (0. 25 μm × 0. 32 mm ×30 m) elastic quartz capillary column; injection port temperature 220 ℃, FID detector temperature 220 ℃, temperature programmed, starting temperature 110 % , keep for 10 min, at 25 ℃ to 230 ℃ , temperature programmed to keep 9.2 min, diversion ratio 10: 1, including 1 L sample quantity. Result: The autumn lee alcohol, ketone of patchouli, thymol, sweet fineleaf schizonepeta herb phenol concentration in sample quantity is 1. 109-0. 110 9, 0. 504-0. 050 4, 0. 987-0. 098 7, 0. 605-0. 060 5 g·L^-1 and good linear relationship between peak area, linear relationship is Y=1 653.05X-1.46 (r=0.999 8), Y=1 207.45X-16.10 (r=0.9997), Y=1 691.68X- 18.06 (r=0.9995), Y=1 547.18X+5.55 (r=0.999 6) sample recovery rate was 99. 9%-103.7% (n =9)98.4% -104.4%, 104.4%-101.4% and 101.4%-97.2%, RSD was 1.9%, 2.3%, 2.5% and 1.9% respectively. Conclusion: The optimized method has good separating degree, negative without interference, easy operation, stable and feasible.
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