顶空气相色谱法测定地奈德中有机溶剂残留量

Determination of residual solvents in desonide by headspace GC

目的：建立顶空气相色谱法测定地奈德中有机溶剂残留量。方法：采用Agilent DB-WAX毛细管柱（30 m×0.25 mm,0.50μm）;氮气为载气,流速为1.5 ml/min;分流比为5∶1;进样口温度为200℃;FID检测器,检测器温度为250℃;程序升温：初始温度40℃,保持10 min,然后以20℃/min升温至200℃,保持5 min。顶空进样,平衡温度为80℃,平衡时间为25 min;以二甲基亚砜为溶剂,外标法测定地奈德中甲醇、乙醇、丙酮、乙酸乙酯、乙醚和三氯甲烷的残留量。结果：甲醇、乙醇、丙酮、乙酸乙酯、乙醚和三氯甲烷均能得到良好的分离,空白溶剂无干扰,检测浓度在所考查的范围内与峰面积具有良好的线性关系（r=0.999 2~0.999 9）;平均回收率为98.4%~100.6%,甲醇、乙醇、丙酮、乙酸乙酯、乙醚和氯仿检测限分别为0.30、0.50、0.15、0.15、0.05和0.60μg/ml。结论：本试验建立的色谱方法简便、准确,适合地奈德原料中有机溶剂残留量的检测。

Objective： To establish a method of headspace capillary gas chromatography for the determination of residual solvents in desonide. Methods： The residual solvents in desonide were separated by Agilent DB- WAX capillary（ 30 m × 0. 25 mm,0. 50μm） column with an FID detector. Nitrogen was used as carried gas and the flow rate of the gas was 1. 5 ml /min. The injector temperature and the detector temperature were controlled at 200 ℃ and 250 ℃,respectively. The programmed column temperature was maintained at 40 ℃ for 10 min and then raised to 200 ℃ at the rate of 20 ℃ / min followed by holding for 5 min. Dimethyl sulfoxide（ DMSO） was used as solvent. The containers of headspace injector were balanced at 80 ℃ for 25 min. Results： The detected solvents were separated completely. The calibration curve of each solvent showed a good linear relationship（ r = 0. 999 2 ~0. 999 9） with good precision and accuracy. The average recovery was in the range of 98. 4% ~ 100. 6%. The LOD of methanol,ethanol,acetone,ethyl acetate,diethyl ether and trichloromethane was 0. 30、0. 50、0. 15、0. 15、0. 05 和 0. 60 μg / ml,respectively. Conclusion： The established method is both simple and accurate,and can be used for the determination of residual solvents in desonide.