GC法检测氯法拉滨中有机溶剂的残留量

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。

Determination of Residual Organic Solvents in Ciofarabine by GC

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.