摘要
目的建立毛细管气相色谱法测定帕司烟肼中的残留溶剂乙醇和异丙醇的含量。方法采用气相色谱法测定,色谱柱为Agilent DB-624毛细管色谱柱（30.0 m×0.32 mm×1.4μm）,载气为氮气,FID检测器,采用顶空进样,程序升温,按外标法计算残留溶剂含量。结果乙醇和异丙醇分别在50.66~151.97μg/m L和49.23~147.69μg/m L范围内呈良好的线性关系（r=0.999 9,n=5）;乙醇、异丙醇加样回收率分别达到99.7%、99.5%;仪器精密度高,乙醇、异丙醇峰RSD均为1.0%（n=6）;稳定性好,24 h间隔进样乙醇、异丙醇峰面积RSD分别为0.86%、0.14%。结论本方法简单、灵敏、可靠,适用于帕司烟肼中残留溶剂的分析检测。
OBJECTIVE To establish a method of head-space capillary gas chromatography（ CGC） for the determination of residual solvents of ethanol and iso-Propyl alcohol in pasinizide. METHODS The residual solvents in pasiniazid were separated by Agilent DB-624 capillary column（ 30.0 m×0.32 mm×1.4 μm） with head-space sampling and temperature programmed. The carried gas was nitrogen. FID was detector. The contents of residual solvents were calculated by external standard method. RESULTS Linearofethanol and iso-Propyl alcohol were good in their ranges of 50. 66- 151. 97 μg / mL and 49. 23- 147. 69 μg / mL（ r = 0. 999 9,n = 5）,respectively. The average recoveries of ethanol and iso-Propyl alcohol were 99. 7% and 99. 5%. The method was with high instrument precision,and RSD of ethanol and iso-Propyl alcohol were both 1.0%（ n = 6）. The method was stable,RSD of ethanol and iso-Propyl alcohol injected in 24 h were 0.86% and 0.14%. CONCLUSION The developed method is simple,sensitive and accurate for the residual solvent analysis of pasiniazide.
出处
《今日药学》
CAS
2016年第4期245-247,共3页
Pharmacy Today
关键词
气相色谱法
残留溶剂
帕司烟肼
gas chromalography
residual solvents
pasiniazide
