摘要
目的建立同时测定拉帕替尼原料药中乙醇、丙酮、异丙醇、二氯甲烷、四氢呋喃、甲苯、N,N-二甲基甲酰胺7种有机溶剂残留量的顶空气相色谱法。方法色谱柱为Agilent DB-624毛细管柱(30 m×0.32 mm,1.8μm),检测器为氢火焰离子化检测器,程序升温,进样口温度为200℃,检测器温度为200℃,载气为氮气,流速为2.0 m L/min,分流比为10∶1,进样方式为顶空进样,顶空平衡温度为80℃,平衡时间为35 min,进样量为5 m L。结果乙醇、丙酮、异丙醇、二氯甲烷、四氢呋喃、甲苯、N,N-二甲基甲酰胺7种残留有机溶剂均完全分离,空白溶剂无干扰;各对照品均在各自的质量浓度范围内与峰面积线性关系良好;精密度、稳定性、重复性试验的结果均符合要求;7种有机溶剂的平均加样回收率为98.22%~98.73%,RSD为0.71%~1.31%(n=9)。结论该方法操作简便,结果准确,重复性好,可用于同时测定拉帕替尼原料药中7种有机溶剂的残留量。
Objective To establish a headspace gas chromatography method for the simultaneous determination of ethanol,acetone,isopropanol,dichloromethane,tetrahydrofuran,toluene and N,N-dimethylformamide in lapatinib raw materials.Methods The chromatographic column was Agilent DB-624 capillary column(30 m×0.32 mm,1.8μm),the detector was flame ion detector(FID)with programmed temperature,the temperature of injection port was 200℃,the temperature of FID was 200℃,the carrier gas was nitrogen,the flow rate was 2.0 mL/min,the split ratio was 10∶1,the injection mode was headspace injection,the temperature of headspace equilibration was 80℃,the equilibration time was 35 min,and the injection volume was 5 mL.Results The seven kinds of organic residual solvents(ethanol,acetone,isopropanol,dichloromethane,tetrahydrofuran,toluene and N,N-dimethylformamide)were completely separated,and the blank solvent had no interference.There was a good linear relationship between the peak area and the concentration of each reference substance.The results of precision,stability and repeatability tests all met the requirements.The average recoveries of seven organic solvents were in the range of 98.22%-98.73%with RSDs of 0.71%-1.31%(n=9).Conclusion The method is simple,accurate and reproducible,which can be used for the simultaneous determination of seven residual organic solvents in lapatinib raw materials.
作者
付丙月
王金虎
王颖超
段崇刚
FU Bingyue;WANG Jinhu;WANG Yingchao;DUAN Chonggang(Shandong Academy of Pharmaceutical Sciences·Shandong Provincial Key Laboratory of Chemical Drugs,Jinan,Shandong,China 250011)
出处
《中国药业》
CAS
2021年第15期62-65,共4页
China Pharmaceuticals
基金
山东省重大科技创新工程和结转项目[2019JZZY010520]。
关键词
拉帕替尼
原料药
顶空气相色谱法
有机溶剂
残留量
同时测定
lapatinib
raw materials
headspace gas chromatography
organic solvents
residual amount
simultaneous determination
