毛细管气相色谱法测定葛根素中乙醇及乙酸残留量

Capillary gas chromatographic determination of residual ethanol and acetic acid in puerarin

目的:建立葛根素中乙醇及乙酸残留量的测定方法。方法:采用直接进样毛细管气相色谱法,色谱柱是以硝基对苯二酸改性的聚乙二醇(DB-FFAP)为固定相的石英毛细管柱(0.32mm×30m,0.25mm),以二氧六环为溶剂,柱温采用程序升温,载气为氮气,流速2.0ml/min,采用氢离子火焰检测器,温度为300℃,进样口温度150℃,分流比25:1,进样量1ml。结果:2种溶剂分离良好,在10mg/L到90mg/L的质量浓度范围内各自峰面积与质量浓度呈良好的线性关系;加样回收率、进样精密度、溶液稳定性令人满意。结论:该方法简便、快速、专属性强、准确度高,可用于原料药中乙醇及乙酸残留量的测定。

Aim ： To determine the residual amounts of ethanol and acetic acid in puerarin. Methods： A capillary gas chromatographic method with directly sampling was employed. The analytical column was DB-FFAP （0.32 mm × 30 m, 0.25 mm） capillary quartz column. The samples were dissolved in 1,4-dioxane. The column temperature was programmed. The carrier gas was nitrogen and its flow-rate was 2.0 ml/min. The detector was FID and its temperature was 300℃. The injector temperature was 150℃ , the split ratio was 25 ： 1, and the injection volume was 1 ml. Results： The linear ranges of ethanol and acetic acid were both from 10 mg/L to 90 mg/L. The results of recoveries, precisions of continuously injections and the solution stability were all satisfactory. Conclusion： The method is simple, rapid, specific and precise. It could be used for the determination of residual amounts of ethanol and acetic acid in drug substances.