摘要
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。
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.
出处
《中国药业》
CAS
2008年第11期26-27,共2页
China Pharmaceuticals
