c-Met抑制剂SPH3348原料药残留溶剂测定法  

Determination of the solvent residue in c-Met inhibitor SPH3348 by capillary gas chromatography

作　　者：孙雨婷 叶小辉 万初东 崔艳[1] SUN Yuting;YE Xiaohui;WAN Chudong;CUI Yan(Shenyang Pharmaceutical University,Shenyang 110016,China;Shanghai Pharma Group(Benxi)Northern Pharmaceuticals Co.,Ltd.,Benxi 117004,China)

机构地区：[1]沈阳药科大学,辽宁沈阳110016 [2]上海医药集团(本溪)北方药业有限公司,辽宁本溪117004

出　　处：《沈阳药科大学学报》2023年第3期287-292,共6页Journal of Shenyang Pharmaceutical University

摘　　要：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=0.9991~0.9998),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,1.8μm)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=0.9991-0.9998).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：SPH3348原料药 残留溶剂 气相色谱法 内标法 

分 类 号：R917[医药卫生—药物分析学]