孙雨婷,叶小辉,万初东,崔艳
SUN Yuting,YE Xiaohui,WAN Chudong,CUI Yan

• 1:沈阳药科大学
• 2:上海医药集团(本溪)北方药业有限公司

摘要(Abstract)：

目的 为测定c-Met抑制剂SPH3348原料药中7种残留溶剂，从而建立顶空-毛细管柱气相色谱内标法。方法 色谱柱为安捷伦DB-624毛细管柱(60 m×0.32 mm, 1.8μm),检测器为氢火焰离子化检测器，载气为氮气，采用程序升温方式进行检测。稀释溶剂为1,3-二甲基-2-咪唑啉酮，选用的内标物为正丙醇，测定SPH3348原料药中残留溶剂。结果 7种有机溶剂(甲醇、乙醇、二氯甲烷、乙酸乙酯、正丁醇、二氧六环、二甲基甲酰胺)分离度均大于1.5,进样浓度与峰面积线性关系良好(r=0.999 1～0.999 8),加样回收率为92.9%～104.1%。结论 本方法可用于测定SPH3348原料药残留溶剂。
Objective To develop a capillary gas chromatography method for determination of seven kinds of residual solvents in c-Met inhibitor SPH3348 substance.Methods The samples were injected into Agilent DB-624 capillary column(60 m×0.32 mm, 1.8 μm) and analyzed with FID detector.Nitrogen was used as carrier gas with headspace injection.Dimethyl imidazolinone was used as solvent and N-Propanol was used as the internal standard.Results The resolutions of the seven organic solvents of methanol, ethanol, dichloromethane, ethyl acetate, n-butanol, dioxane and dimethylformamide were more than 1.5.There were good linear relationships in the experimental concentrations(r=0.999 1-0.999 8).The average recoveries were ranged from 92.9%-104.1%.Conclusion The method can be used for detection of residual solvents in c-Met inhibitor SPH3348.

关键词(KeyWords)： SPH3348原料药;残留溶剂;气相色谱法;内标法
SPH3348;solvent residue;capillary gas chromatography;internal standard method

Abstract:

Keywords:

基金项目(Foundation):

作者(Author): 孙雨婷,叶小辉,万初东,崔艳
SUN Yuting,YE Xiaohui,WAN Chudong,CUI Yan

DOI: 10.14066/j.cnki.cn21-1349/r.2021.0184

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