他克莫司原料药中残留溶剂检测方法研究.pdfVIP

  他克莫司原料药中残留溶剂检测方法的研究 * 陈忠 连云阳 魏宗有 范建辉 （福建省微生物研究所，福州 350007 ） 摘要 目的：建立他克莫司原料药中的有机溶剂残留量检测方法。方法：采用气相色谱法，色谱 柱为弹性石英毛细管柱（6%腈丙基苯基—94%二甲基聚硅氧烷为固定液），进样口温度 170℃；火焰 离子化检测器（FID ）温度：250 ℃；柱温：程序升温，初始温度 60℃，维持 6 分钟，以 25 ℃/min 的速率升温至 220 ℃，维持 4.6 分钟。；载气：氮气，进样方式：分流进样，分流比：30:1 ；柱压力 12KPa。以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 该法可用于他克莫司原料药中有机溶剂残留量检测。 关键词：他克莫司；残留溶剂；气相色谱 GC detection of residual solvents in Tacrolimus * Chen Zhong, Lian Yun-yang ，Wei Zong you, Fan Jian-hui (Fujian Institute of Microbiology, Fuzhou 350007) Abstract: Objective To establish a method for determination of the residual solvents in tacrolimus API. Method The residual solvents in tacrolimus were determined by GC using a capillary column (6% phenyl nitrile and 94% two methyl polysiloxane as stationary liquid) with a FID detector, and nitrogen gas was employed as the carrier. The injector inlet and the detector temperature were set at 170℃ and 250 ℃, respectively. The column temperature was kept at 60 ℃ initially for 6 min, then raised to 220 ℃ at a rate of 25 ℃/min and maintained for 4.6 min. Split injection at a ratio of 30:1 was performed under the pressure of 12KPa, and external standard method was adopted using dimethylacetylamide as solvent. Results and Conclusion The established method demonstrated high resolution and good linear relationship between peak area and concentration of the residual solvents, and is reliable and applicable for detection of the residual solvents in tacrolimus API. Key words: tacrolimus; residual solvents; GC 他克莫司(Tacrolimus) 又名 FK506 ，1984 年是