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顶空气相色谱法测定硝唑尼特中的残留溶剂
Determination of Residual Solvents in Nitazoxanide by Headspace Gas Chromatography
【摘要】 目的:建立项空气相色谱测定药物硝唑尼特中残留溶剂的方法。方法:采用DM-WAX毛细管色谱柱(30 m×0.25 mm,0.5μm);枉温采取程序升温;进样口温度为200℃;FID检测器,检测器温度为250℃;顶空进样,平衡温度为80℃,平衡时间为30 min;以N,N-二甲基甲酰胺为溶剂测定硝唑尼特原料药中丙酮、二氯甲烷的残留量。结果:在本文的色谱条件下,各有机溶剂均能得到有效分离,丙酮、二氯甲烷的浓度分别在250~750μg·ml-1(r=0.999 1)、30~90μg·ml-1(r=0.999 1)范围内线性关系良好;平均回收率分别为99.15%、99.18%,RSD分别为2.17%、2.97%(n=9)。结论:本方法简便、快速、准确,可有效检测硝唑尼特中的残留溶剂。
【Abstract】 Objective:To establish a method for the determination of residual solvents in nitazoxanide by headspace gas chromatography. Method:The residual solvents in nitazoxanide were separated by a DM-WAX column(30 m×0.25 mm,0.5μm) with an FID detector.The injector temperature and the detector temperature was set at 200℃and 250℃,respectively.The containers of head-space injector were in equilibrium at 80℃for 30 min.N,N-Dimethylformamide was used as the solvent.Result:The detected solvents were separated completely.A good linearity of the two solvents was obtained within the range ol 250-750μg?ml(r=0.9991) and 30-90μg?ml-1(r=0.9991),respectively.The average recovery of acetone and dichloromethane was 99.15%and 99.18%will) RSD of 2.17%and 2.97%(n=9),respectively.Conclusion:The established method is simple,rapid and accurate,and can be used in the determination of residual solvents in nitazoxanide.
【Key words】 Nitazoxanide; Residual solvents; Gas chromatography; Acetone; Dichloromethane;
- 【文献出处】 中国药师 ,China Pharmacist , 编辑部邮箱 ,2013年08期
- 【分类号】R927
- 【被引频次】2
- 【下载频次】58