【摘要】 目的:建立以气相色谱法检测氯法拉滨原料药中7种有机溶剂残留量的方法。方法:毛细管柱为AT-1301;载气为氮气;检测器为火焰离子化检测器;柱温采取程序升温,初始温度40℃,以7℃.min-1升至80℃,再以20℃.min-1升至200℃,保持2min;进样口温度250℃;检测器温度280℃;分流直接进样。检测3批氯法拉滨原料药中甲醇、乙腈、二氯甲烷、叔丁醇、乙酸乙酯、正庚烷、乙酸的残留量。结果:各有机溶剂均能得到有效分离,在所考察的浓度范围内线性关系良好(r=0.99941～0.99993),平均回收率为96.5%～102.4%,RSD均小于4.0%,3批样品中7种有机溶剂残留量均符合《中国药典》要求。结论:本方法灵敏、准确、可靠,可用于氯法拉滨原料药中有机溶剂残留量的检测。更多还原

【Abstract】 OBJECTIVE:To establish a gas chromatography(GC)method for determination of seven residual solvents in clofarabine.METHODS:The capillary column was AT-1301;the carrier gas was nitrogen gas and the detector was FID.By temperature programming was applied for the column temperature with an initial temperature of 40 ℃,which rose to 80 ℃ with an increase rate of 7 ℃·min-1,then rose to 200 ℃(kept at this temperature for 2 min)with the increase rate of 20 ℃·min-1.The injector temperature was 250 ℃ and the detector temperature was 280 ℃.The sample was injected directly for determination of residual levels of methanol,acetonitrile,dichlormethane,t-butyl alcohol,ethyl acetate,n-heptane and acetic acid in 3 batches of clofarabine.RESULTS:All the organic solvents were effectively separated and they showed good linearity within a concentration range(r=0.999 41～0.999 93)with average recovery rate ranged from 96.5% to 102.4%(RSDs of all were less than 4.0%).7 kinds of organic solvents in 3 batches of samples were all up to the standard specified in Chinese Pharmacopeia.CONCLUSION:The method is sensitive,accurate and reliable,and it is applicable for the determination of the residual solvents in clofarabine.更多还原