【摘要】 目的:建立同时测定凡德他尼原料药中8种有机溶剂即甲醇、乙醇、四氢呋喃、正己烷、二氯甲烷、乙酸乙酯、异丙醇、N,N-二甲基甲酰胺含量的方法。方法:采用毛细管气相色谱法,以二甲基亚砜(DMSO)为溶剂,按外标法计算溶剂残留量。色谱柱为DB-624,进样口温度为250℃,氢火焰离子化检测器温度为270℃,程序升温,载气为N2,分流比为20∶1。结果:8种有机溶剂在各自的检测质量浓度范围内线性关系良好(r=0.998 1~0.999 4);平均加样回收率为95.90%~101.4%(RSD=0.56%~3.16%,n=3);3批样品中有1批检出四氢呋喃和N,N-二甲基甲酰胺。结论:建立的方法操作简单、灵敏、结果准确,可用于凡德他尼原料药中有机溶剂残留量检查。更多还原

【Abstract】 OBJECTIVE:To develop a method for the content determination of 8 residual organic solvents as methanol,ethanol,tetrahydrofuran,n-hexane,dichlormethane,ethyl acetate,isopropanol,N,N-dimethylformamide in vandetanib raw material.METHODS:Gas chromatography method was adopted using DMSO as solvent. The contents of residual solvent were determined by external standard method. The determination was performed on DB-624 column with FID detector. The injector temperature was set at 250 ℃ and the detector temperature was 270 ℃ by temperature programming. Carrier gas was nitrogen,and the splitting ratio was 20 ∶ 1. RESULTS:The good linear relation of 8 kind of organic solvents were achieved(r=0.998 1-0.999 4). The average recoveries were ranged from 95.90% to 101.4%(RSD=0.56%-3.16%,n=3). Among 3 batches of samples,tetramethylene oxide and N,N-dimethylfomamide were detected in 1 batch of sample. CONCLUSIONS:The method is simple,sensitive and accurate,and can be used for the determination of residual organic solvents in vandetanib raw material.更多还原