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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

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【作者】 张建业; 可钰; 阎学斌; 刘宏民;

【Author】 ZHANG Jianye, KE Yu, YAN Xuebin, LIU Hongmin New Drug Research and Development Center, Zhengzhou University; Department of Chemistry, Zhengzhou University, Zhengzhou 450052

【机构】 郑州大学新药研究开发中心郑州大学化学系; 郑州大学新药研究开发中心郑州大学化学系 郑州450052; 郑州450052; 郑州450052;

【摘要】 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。

【Abstract】 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 25GA6FA1, 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.

  • 【文献出处】 郑州大学学报(医学版) ,Journal of Zhengzhou University(Science Medical) , 编辑部邮箱 ,2005年05期
  • 【分类号】R284
  • 【被引频次】2
  • 【下载频次】291
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