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毛细管气相色谱法检测多潘立酮中的残留溶剂

Capillary gas chromatographic determination of residual solvents in domperidone

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【作者】 段东红康玉英刘世斌

【Author】 DUAN Dong-hong~1 KANG Yu-ying~2 LIU Shi-bin~1 (1.College of Chemical Engineering &Technology of Taiyuan University of Technology,Shanxi,Taiyuan 030024,China;2.Taiyuan Center Hospital,Shanxi,Taiyuan 030009,China)

【机构】 太原理工大学化学工程与技术学院太原市中心医院

【摘要】 目的:建立气相色谱法检测多潘立酮原料药物中的有机残留溶剂二氯甲烷、氯仿、甲苯、二甲基甲酰胺。方法:色谱柱为 QC2/BP1(25 m×0.22 mm,0.25 μm),载气为氢气,采用氢离子火焰检测器,进样器温度为160℃,检测器温度为260℃,柱温采用二阶程序升温(50℃,保持5 min,以2℃·min-1升至120℃,再以30℃·min-1升至260℃,保持10 min),以二甲基亚砜为溶剂,进样量1 μL。结果:二氯甲烷、氯仿、甲苯、二甲基甲酰胺的线性关系 r 分别为0.9999,0.9998,0.9998,0.9994。平均回收率(n=5)分别为99.3%,97.6%,101.5%,96.9%;RSD 分别为2.0%,2.8%,2.5%,3.2%。结论:方法柱效高、灵敏、准确,适用于同时检测多潘立酮原料药物中二氯甲烷、氯仿、甲苯和二甲基甲酰胺的含量。

【Abstract】 Objective:To establish a GC method for determination of methylene chloride,chloroform,toluene and dimethyl-formylamine in domperidone by capillary gas chromatographic.Method:A column QC2/BP1,25m× 0.22mm was adopted.The injector temperature was 160℃,the detector temperature was 260℃,the column tem- perature is gradiently raised with initial temperature at 50℃,sustained for 5min,then raised to 120℃ at the rate of 2℃·min-1,then raised to 260℃Cat the rate of 30℃·min-1,sustained for 10min.The solvent was dimethyl sul- foxide.Results:The correlation factors r in methylene chloride,chloroform,toluene and dimethyl-formylamine was 0.9999,0.9998,0.9998 and 0.9994 respectively.The recovery(n=5)was 99.3%,97.6%,101.5% and 96.9% with RSD 2.0%,2.8%,2.5% and 3.2%,respectively.Conclusion:The method appeared to be sensitive and ac- curate,and can be used for the determination of the residual organic solvent in domperidone.

  • 【文献出处】 药物分析杂志 ,Chinese Journal of Pharmaceutical Analysis , 编辑部邮箱 ,2006年04期
  • 【分类号】R927
  • 【被引频次】1
  • 【下载频次】65
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