{Author}:林燕琴 陈 忠 徐敏华 赵学清 章卫忠 陈志航

　　{Year}:2013

　　{Title}:顶空气相色谱法测定氯法拉滨中有机溶剂残留量

　　{Journal}:《今日药学》

　　{Volume}:23

　　{Issue}:11

　　{Pages}: 727-729

　　{ISBN/ISSN}: 1674-229X

　　{Keywords}:氯法拉滨 残留溶剂 顶空气相色谱

　　{Abstract}:目的建立顶空气相色谱法测定氯法拉滨中有机溶剂残留量。方法采用Agilent DB-624弹性石英毛细管柱(30 m×0.53 mm,3.0μm),火焰离子化检测器(FID),载气为氮气;进样口温度170℃;检测器温度:300℃;分流比:30∶1;柱压力12 kPa;柱温:程序升温,初始温度40℃,维持1 min,以15℃/min的速率升温至250℃,维持1 min。顶空进样,平衡温度为80℃,平衡时间30 min。以N,N-二甲基乙酰胺为溶剂,外标法测定。结果被测物均能得到很好的分离,峰面积与浓度呈良好的线性关系,精密度良好。结论该法简便、准确、灵敏度高,可用于氯法拉滨有机溶剂残留量检测。

　　Objective To establish a method of headspace gas chromatography for the determination of the residual solvents in Clofarabine. Methods The Agilent DB-624 capillary column( 30 m × 0. 53 mm,3. 0μm) with an flame ionization detector( FID) was adopted,and nitrogen gas was used as carrier. The temperatures of the injector inlet and the detector were set at 170 ℃ and 300 ℃,respectively; Split injection was excuted at a ratio of 30 ∶ 1 under the pressure of 12 kPa; The program of the column temperature.