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顶空气相色谱法测定替加氟中残留的有机溶剂

Determination of Residual Organic Solvents in Tegafur by Headspace Gas Chromatography

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【作者】 周丽英游慧刘江华

【Author】 Zhou Laying,You Hui,Liu Jianghua(Yangzte River Pharmaceutical Group Co.,Ltd.,Jiangsu Taizhou 225321,China)

【机构】 扬子江药业集团有限公司药物研究院

【摘要】 目的:建立顶空气相色谱法测定替加氟中4种有机溶剂残留量的方法。方法:顶空进样程序升温,色谱柱为HP-IN-NOWAX(30.0 mm×0.32 mm×0.50μm),溶剂为二甲亚砜(DMSO),检测器为FID,载气为氮气。结果:4种有机溶剂完全分离,在所考察的浓度范围内线性关系良好,甲醇、乙醇、三氯甲烷、N,N-二甲基甲酰胺(DMF)的最低检出浓度分别为0.299,0.100,3.060,1.850μg·ml-1。结论:该方法简便灵敏,结果准确可靠,适用于替加氟原料中有机溶剂残留量的检测。

【Abstract】 Objective:To establish a headspace gas chromatography method for determining the residual organic volatile solvents in Tegafur.Method:The samples were injected by a headspace sampler under temperature programmed heating.The determination was performed on an HP-INNOWAX capillary column(30.0 mm×0.32 mm,0.50μm) while DMSO was used as solvent media,FID as detector and nitrogen as carrier gas.Result:The four residual organic solvents consisting of methanol,ethanol,chloroform and DMF were completely separated,and the linear relationships were promising.Their minimal detective levels was 0.299,0.100,3.060 and 1.850μg·ml-1,respectively.Conclusion:The method is simple,sensitive,accurate,and can be used for detection of four residual solvents in Tegafur.

  • 【分类号】R927.1
  • 【被引频次】1
  • 【下载频次】64
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