气相色谱法测定雌激素化合物S21中的残留溶剂

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。

Determination of residual solvents in estradiol S21 by GC

To establish a method for determining the residues of four kinds of solvents in S21 by capillary gas chromatography.The capillary column was DB-Wax(30 m×0.45 mm, 0.85μm)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 50℃(hold 5min)and increased at the rate of30℃/min to 200℃(hold 7min),The sample was dissolved in N,N-dimethylformamide and acetonitrile 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 0.9997～0.9999). The rate of recovery was in the range of 97%-～100%.The numberof 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.