气相色谱法测定雌激素化合物S21中的残留溶剂  

Determination of residual solvents in estradiol S21 by GC

作　　者：刘琳[1] 肖炳坤[1] 杨建云[1] 黄荣清[1] 

机构地区：[1]军事医学科学院放射与辐射医学研究所,北京100850

出　　处：《现代仪器》2011年第2期52-54,共3页Modern Instruments

基　　金：国家科技重大专项"重大新药创新"综合性新药研究开发技术大平台(2009ZX09301-002);国家自然科学基金项目(NO 81072613)

摘　　要：用毛细管气相色谱法建立S21中4种残留溶剂的测定方法。采用DB-Wax(30m×0.45mm,0.85μm)毛细管柱,载气为氮气,FID检测器。采用程序升温,柱温:起始温度为50℃,保持5min,然后以30℃/min的速率升至200℃,保持7min。进样口温度:250℃,检测器温度:250℃。分流直接进样,N,N-二甲基甲酰胺为溶剂,乙腈为内标物,内标法测定残留溶剂的含量。在考察范围内呈良好的线性关系(乙醇r=0.9997,丙酮r=0.9997,乙酸乙酯r=0.9998,甲苯r=0.9999),平均回收率为97%～100%,理论塔板数大于10000,相邻峰分离度均大于2,精密度、重复性的RSD均小于3%。本法简单、结果准确、重复性好,适用于S21中乙醇、丙酮、乙酸乙酯、甲苯4种残留溶剂的同时检测。To establish a method for determining the residues of four kinds of solvents inS1 by capiilary gas chromatography, capillary coiumn was DB-Wax（30 m × 0.45 mm,0.85μm） with an FID detector and nitrogen as carrer gas. The injector temperature and the detector temperature were both controlled at250℃,respectively .The column temperature program was initially 50℃（hold 5min）and increased at the rate of 30℃/min to 200℃（hold 7min）,The sample was dissolved in N,N-dimethylformamide and acetonitrile was used as the imternal standard .The assay of residual solventswas calculated by intemal standard method .A good linearity was observed at the experimental concentration（r 0.9997-0.9999）.The rate of recovery was in the range of 97%-100%.The number of theoreticalplates ecceeded 10000 and the resolutions between the adjacent peaks were more than 2.The RSD of precision and accuracy was less than 3%.The method is simple ,sensitive ,accurate,and can be used for detection of four residual solvents in Colpolrophine

关 键 词：气相色谱法 雌激素 残留溶剂 内标法 

分 类 号：O657.71[理学—分析化学]