摘要
Abstract
OBJECTIVE: To establish the method for the content determination of 4 kinds of residμal organic solvents (metha-nol, ethanol, N, JV-dimethylformamide, dimethylsμlfoxide) in clobetasol propionate. METHODS: The residμal solvents in beclo-metasone dipropionate were separated on HP-INNOWAX capillary colμmn. 1,6-dioxane was μsed as solvent. The carried gas was nitrogen at flow rate of 1.0 Ml-min-1. The programmed colμmn temperatμre was set as follows: maintained at 60 ℃ for 5 min and raised to 160 ℃ at the rate of 30 t ·min-1 followed by holding for 5 min. The injector temperatμre and FID detector temperatμre were controlled at 160 t and 250 X., respectively. The splitting-ratio was 5.0:1. Hydrogen was μse as fμel gas at flow rate of 30 Ml'inin-1 with air as combμstion-sμpporting gas at flow rate of 450 Ml-min-1. The makeμp gas was nitrogen at flow rate of 25 Ml-min-1. The injection volμme was 1 Μl. The contents of 4 kinds of residμal solvents in 5 batches of samples were determined μnder same condition. RESULTS: Methanol, ethanol, JV.JV-dimethylforrnamide, dimethylsμlfoxide in clobetasol propionate were completely separated. The linear ranges were 0.02 - 1.0 g-L-1 (r= 1.000). Average recovery rates were 97.6% -102.5% (RSD< 2.88%). The minimμm qμantitative concentrations were 0.60 μg·Ml-1,0.98 μg"Ml-1,0.38 μg·Ml-1, 0.85 μg-Ml-1,respectively. Methanol was foμnd in 1 batch of sample and ethanol was foμnd in 2 batches of samples. No organic solvent was foμnd in other batches of samples. CONCLUSIONS: The established method is proved to be accμrate and sensitive. It can be μsed for simμltaneoμs determination of 4 kinds of residμal organic solvents in clobetasol dipropionate.关键词
毛细管气相色谱法/丙酸氯倍他索/残留有机溶剂Key words
Capillary gas chromatography/Clobetasol propionate/Residμal solvents分类
医药卫生
