摘要
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, 3.0 μm） 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 rising was set as initialing at 40℃ with maintenance for 1 min, then rising to 250℃ at a rate of 15℃/min and maintaining for 1 min. Samples in the injector were equilibrated at 80℃ for 30 min. External standard method was used with dimethylacetylamide as a solvent. Results Excellent resolution and good linear cablibration curves of the residual solvents were obtained. Conclusion The brief, accurate and sensitive method can be applied in the detection of residual solvents in Clofarabine.
出处
《今日药学》
CAS
2013年第11期727-729,共3页
Pharmacy Today
基金
2011年福建省区域科技重大项目资助(编号:2011Y3001)
关键词
氯法拉滨
残留溶剂
顶空气相色谱
clofarabine
residual solvents
headspace gas chromatography
