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

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

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g（30m×0．53mm×3μm），以N2为载气，FID检测器，程序升温。结果DMF在8．83×10～176．6×10^-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。

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 min ×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 netilmiein sulfate .