摘要
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.
作者
丁邦东
龚爱琴
DING Bangdong;GONG Aiqin(Yangzhou Polytechnic Institute,Yangzhou 225127,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2018年第6期1032-1035,共4页
Chemical Research and Application
基金
2016年江苏省‘青蓝工程’项目(苏教师﹝2016﹞15号)资助
2016年扬州工业职业技术学院校级科研课题(2016xjzk008)资助
关键词
醋酸氢化可的松
残留溶剂
气相色谱
hydrocortisone acetate
residual organic solvent
gas chromatography