气相色谱法测定雄烯二醇中的残留溶剂  

Determination of Residual Solvents in Androstendiol by Gas Chromatography

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：《现代科学仪器》2011年第2期78-80,共3页Modern Scientific 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雄烯二醇7种残留溶剂的测定方法。采用DB-Wax(30m×0.45 mm,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45℃,保持10min,然后以20℃/min的速率升至140℃,保持10分钟。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,丙酮为内标物,内标法测定残留溶剂的含量。在考察的范围内呈良好的线性关系(乙醇r=0.9997﹑吡啶r=0.9999﹑乙酸乙酯r=0.9993﹑甲苯r=0.99957﹑甲醇r=0.99997﹑二氯乙烷r=0.99995﹑乙酸r=0.9993),样品加标回收率为100.1%～102.8%,理论塔板数大于10000,相邻峰的分离度均大于1.5,精密度﹑重复性的R SD均小于3%。本法简单,结果准确,重复性好,适用于雄烯二醇中乙醇、吡啶、甲苯、乙酸、二氯乙烷、甲醇、乙酸乙酯7种残留溶剂的同时检测。To establish a method for determining the residues of seven kinds of solvents in androstendiol by capillary gas chromatography.The capillary column was DB-Wax（30 mx0.45 mm, 0.85ktm） with an FID detector and nitrogen as carrier gas. The injector temperature and the detector temperature were both controlled at250℃, respectively. The column temperature program was initially 45℃（hold 10min） and was increased at the rate of 20℃/min to 140℃（hold 10min）. The sample was dissolved in N,N-dimethylformamide and acetone was used as the internal standard. The assay of residual solventswas calculated by internal standard method.A good linearity was observed at the experimental concentration （r： 0. 9993-0.9999）. The rate of recovery was in the range of 100.1% -102.8%. The number of theoreticalplates ecceeded 10 000 and the resolutions than 3%.The method is simple, sensitive, accurate, and can be used for detection of seven residual solvents in androstendiol.

关 键 词：气相色谱法 雄烯二醇 残留溶剂 内标法 

分 类 号：TQ460.1[化学工程—制药化工]