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.%目的:建立丙酸氯倍他索原料药中4种有机溶剂（甲醇、乙醇、N,N-二甲基甲酰胺、二甲亚砜）残留量的检测方法.方法:采用毛细管气相色谱法.色谱柱为HP-INNOWAX石英毛细管柱；溶剂为1,6-二氧六环；程序升温,初始温度60℃,保持5min,并以30℃·min-1速率升温至160℃,保持5min；载气为高纯氮气,流速为1.0 mL·min-1;氢火焰离子化检测器温度为250℃；进样口温度为160℃；进样方式为分流进样,分流比为5.0:1；燃气为氢气,30 mL·min-1；助燃气为空气,450 mL·min-1；尾吹气为氮气,25mL·min-1；进样量为1μL.在同一条件下检测5批样品中4种溶剂残留量.结果:甲醇、乙醇、N,N-二甲基甲酰胺、二甲亚砜均能达到完全分离,检测浓度线性范围均为0.02～1.0 g·L-1(r= 1.000)；平均回收率为97.6％～102.5％,RSD小于2.88％；最低定量限分别为0.60、0.98、0.38、0.85 μg·mL-1；5批样品中有1批检测出甲醇,2批中检测出乙醇,其余均未检测出有机溶剂.结论:该方法灵敏、准确,可同时检测丙酸氯倍他索原料药中4种残留有机溶剂.
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