摘要
建立3-氯代亚甲基-6-氟-硫色满-4-酮原料药中甲酸乙酯等残留溶剂的测定方法。采用气相色谱直接进样法,FID检测器,DB-624毛细管柱（30 m×0.45 mm×2.55μm）,应用程序升温,进样口温度180℃,检测器温度200℃,载气为N2,以N,N-二甲基甲酰胺为溶剂,采用外标法定量。在此色谱条件下,4种残留溶剂均能得到较好的分离,空白对照无干扰,各溶剂质量浓度与峰面积具有良好的线性关系（r=0.9990～0.9994）,平均回收率为100.48%～118.22%。建立的方法简单、可靠、精确,可用于3-氯代亚甲基-6-氟-硫色满-4-酮原料药残留溶剂的测定。
A GC method was established for determination of residual solvents of ethyl formate, dichlormethane, n - hexane, and ethyl acetate in the drug substance of 3 - （ chloromethylene ） - 6 - fluoro - thiochroman - 4 - one. The analytieal column was DB -624 （30 m × 0.45 mm × 2.55 μm）. The injector temperature was 180℃ and the detector temperature was 200 ℃. The column temperature was programmed raised. The carrier gas was nitrogen and the solvent was N, N - dimethyl formamide. The residual solvents were quantified with external standard. Under these chromatographic conditions, the detected solvents were well separated. The blank control had no interference. The concentration showed a good linear relationship with the peak areas （ r = 0. 9990 ～ 0.9994）. The average recovery rate was in the range of 100.48% ～ 118.22%. The established method is simple, reliable and accurate for the quantitative determination of residual solvents, and can be used for the quality control of 3 - （chloromethylene） - 6 - fluoro - thiochroman - 4 - one.
出处
《山东化工》
CAS
2016年第3期57-59,共3页
Shandong Chemical Industry
基金
"重大新药创制国家科技"重大专项子课题:3-取代亚甲基硫色满-4-酮抗肿瘤新药研究(2012ZX09103-101-057)
