GC测定舒巴坦匹酯原料药中6种残留溶剂

Determination of the Six Residual Organic Solvents in Sulbactam Pivoxil by GC

目的建立测定舒巴坦匹酯原料药中丙酮、乙酸乙酯、乙醇、二氯甲烷、N,N-二甲基甲酰胺和N,N-二异丙基乙胺6种残留溶剂含量的检测方法。方法采用Rtx-624毛细管柱(30m×0.53mm,3μm),氢离子火焰检测器(FID),进样口温度为180℃,检测器温度为250℃,柱温采用程序升温,载气为氮气;样品溶剂为二甲基亚砜(DMSO),进样量1μL。结果6种有机溶剂均达到完全分离;在考察的浓度范围内线性关系良好,精密度和回收率良好。结论本方法简便、灵敏,结果准确性高,可用于舒巴坦匹酯原料药中残留溶剂的测定。

OBJECTIVE To establish a capillary GC method for the determinat ion of residual organic solvents such as acetone,ethyl acetate,ethanol,dichlo romethane,N,N-dimethylformamide,N,N-diisopropylethylamine in sulbactam piv oxil. METHODS The method was adopted using a Rtx-624 GC column (30m×0.53mm,3μm).FID was used as detector with the temperature of 250℃,a nd the inlet temperature was 180℃.The method used temperature program,nitroge n as carrier gas.The sample was dissolved in DMSO,the injection volume was 1μ L. RESULTS Six residual solvents were separated completely.It was appeared to present a good linearity within the experimental concentration, and the precision and recoveries were good. CONCLUSION The meth od is simple,accurate and highly sensitive,which can be used for the determina tion of the residual solvents in sulbactam pivoxil.