静态顶空-毛细管气相色谱法同时检测氢化可的松中7种微量有机挥发性杂质

Simultaneous Detection of Seven Trace Organic Volatile Impurities in Hydrocortisone by Static Headspace Capillary Gas Chromatography

目的:建立氢化可的松中7种微量有机挥发性杂质同时检测的方法。方法:在0.1 g氢化可的松中加入1 mL的饱和硫酸钠溶液,80℃平衡55 min;顶空采样,气体进样2 mL进行气相色谱分析。结果:7种有机挥发性杂质的回收率都大于90%, 连续6次实验的RSD小于10%。有机挥发性杂质甲醇、乙醇、二氯甲烷、氯仿、苯、三氯乙烯和二氧六环的检测限分别为 0.120,0.060,0.005,0.012,0.001,0.0002,0.152μg·mL-1。结论:该静态顶空-气相色谱分析方法适用于同时检测非挥发性药物的多种有机挥发性杂质。

Objective:To establish a method for simultaneous detection of organic volatile impurities in hydrocorti-sone. Method:1 mL saturated Na2SO4 solution was added in 0.1 g hydrocortisone and the sample was equilibrated at 80℃ for 55 minutes,then 2 mL headspace gas was injected for gas chromatographic assay. Result:The recovery values were higher than 90%.The RSD of continues six analyses was lower than 10%. The detection limit of methanol, ethanol,dichloromethane,chloroform,benzene,trichloroethylene and 1,4-dioxane were 0.120,0.060, 0.005,0.012,0.001,0.0002 and 0.152μg·mL-1 respectively.(Conclusion: This headspace GC method is an ideal technique for simultaneous detection of volatile impurities in non - volatile pharmaceutical matrices.