气相色谱法测定醋酸氢化可的松中残留溶剂含量

Determination of residue organic solvent in hydrocortisone acetate by gas chromatography

本文提出了一种测定醋酸氢化可的松中残留溶剂的气相色谱分析方法。色谱柱为DB-5毛细管柱,采用程序升温的方法,以氮气为载气,用氢火焰离子化检测器(FID)分离测定了醋酸氢化可的松中甲醇、乙醇、丙酮、二氯甲烷、N,N-二甲基甲酰胺(DMF)有机溶剂的残留情况。方法学验证结果表明在实验条件下,甲醇、乙醇、丙酮、二氯甲烷、DMF回收率分别为95.5%、95.0%、94.4%、93.1%、94.2%,定量限分别为1.2、0.75、0.75、1.8、1.7μg·mL^(-1)(信噪比大于10),检测限分别为0.30、0.25、0.25、0.60、0.53μg·mL^(-1)(信噪比大于3),重复性和耐用性实验结果都表明本方法结果准确可靠,可作为醋酸氢化可的松中残留溶剂测定的有效方法。

In this paper a gas chromatography method for determining residual organic solvent in hydrocortisone acetate was developed.DB-5 capillary column with nitrogen gas as carrier and FID as detector was applied in this study. Five residual organic solvents,i.e.methanol,ethanol,acetone,dichloromethane,N,N-dimethylformamide were tested under a gradient temperature. Based on the evaluation-test result,the recoveries of methanol,ethanol,acetone,dichloromethane and N,N-dimethylformamide were 95. 5%,95. 0%,94. 4%,93. 1%,94. 2%,the quantitation limits were 1. 2,0. 75,0. 75,1. 8,1. 7 μg· mL^（-1）,and the detection limits were 0. 30,0. 25,0. 25,0. 60,0. 53 μg · mL^（-1）,respectively. The experimental results of repeatability and durability showed that this method was accurate and reliable and can be used as an effective method for the determination of residual solvent in hydrocortisone acetate.