顶空气相色谱法测定氢化可的松琥珀酸钠中N，N-二甲基甲酰胺的残留量

目的建立测定氢化可的松琥珀酸钠中有机溶剂N，N-二甲基甲酰胺（DMF）残留量的方法。方法采用顶空气相色谱法，色谱柱为DB-624毛细管色谱柱（30m×0．32mm，1．8μm），载气为氮气，分流比为10：1，以二甲基亚砜（DMSO）为溶剂，柱温85℃，保持10min，然后以35℃／min的速率升温至200℃，保持6min，进样口温度为220℃，氢火焰离子化检测器（FID）温度为250℃。结果DMF质量浓度在0．0567～0．5090mg／mL范围内与峰面积线性关系良好，r=0．99998（n=7），平均加样回收率为101．4％，DMF的最低检出限为0．0028％。结论顶空气相色谱法可用于测定氢化可的松琥珀酸钠中有机溶剂DMF的残留量。

Determination of N,N-dimethylformamide in Hydrocortisone Sodium Succinate by Headspace Gas Chromatography

Objective To establish a method to determine N, N-dimethylformamide residues in hydrocortisone sodium succinate. Methods The quantification by the headspace gas chromatography was as follows： using DB-624 capillary column （30 m×0.32 mm,1.8 μm） and FID detector,the analysis was carried out at the split rate of 10 ： 1,nitrogen as carrier gas. DMSO was used as the solvent. The oven temperature was beginning from 85 ℃. After maintaining 10 min,the temperature was programmatically increased to 200 ℃ at the rate of 35 ℃ per min and maintained for 6 min. The injection port temperature was 220 ℃ and the detector temperature was 250 ℃. Results The calibrated linear plot of N,N- dimethylformamide was within 0. 056 7-0. 509 0 mg/mL （r =0. 999 98） with the average recovery rate of 101.4%.The detection limit was 0. 002 8%. Conclusion This sensitive and reliable quantification is favorable to detect the residual solvent N,N- dimethylformamide in hydrocortison sodium succinate.