顶空气相色谱法测定硫酸奈替米星中N,N-二甲基甲酰胺溶剂残留量

目的建立测定硫酸奈替米星中N,N-二甲基甲酰胺(DMF)溶剂残留量的方法。方法采用顶空毛细管气相色谱法,以二甲基咪唑啉酮(DMI)为溶剂,平衡时间为30min,DB-624色谱柱(30m×0.53mm×3μm),以N2为载气,FID检测器,程序升温。结果DMF在8.83×10-3~176.6×10-3g·L-1范围内呈良好的线性关系(r=0.9990),平均回收率为98.7%,RSD为3.3%。结论该方法准确可靠,可作为硫酸奈替米星原料中DMF残留量的控制方法。

Determination of residual N,N-dimethylformamide in netilmicin sulfate by head space gas chromatography

Objective To establish a method for the determination of residual N,N-dimethylformamide(DMF)in netilmicin sulfate. Methods Headspace gas chromatography was established, the chromatographic column was DB-624(30 m×0.53 mm×3 μm),the detector was FID, the carrier gas was N2; the solvent was 1,3-Dimethyl-2-imidazolidinone(DMI) and the equilibrium time was 30 min,temperature was controlled by program. Results The linearity of DMF was good within the range of 8.83×10-3～176.6×10-3 g·L-1(r=0.999 0),The average recovery was 98.7%, with RSD 3.3%( n=6 ). Conclusion This method is accurate, and could be used to control residual N,N-dimethylformamide(DMF)in netilmicin sulfate .