GC法测定3-氯代亚甲基-6-氟-硫色满-4-酮中残留有机溶剂  

Determinatioon of Residual Solvents in 3-(chloromethylene)-6-fluoro-thiochroman-4-one by GC

作　　者：赵静静[1,2] 王利娟[1,2] 安宁[1,2] 吕丽丽[1,2] 郭怀忠[1,2] 

机构地区：[1]河北大学药学院河北省药物质量分析控制重点实验室,河北保定071002 [2]河北大学药物化学与分子诊断教育部重点实验室,河北保定071002

出　　处：《山东化工》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)

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.

关 键 词：气相色谱法 3-氯代亚甲基-6-氟-硫色满-4-酮 乙酸乙酯 N N-二甲基甲酰胺 

分 类 号：O657.71[理学—分析化学]