毛细管气相色谱法测定丙酸倍氯米松中3种有机溶剂残留量

Determination of 3 Kinds of Residual Organic Solvents in Beclometasone Dipropionate by Capillary Gas Chromatography

目的:建立丙酸倍氯米松中3种有机溶剂残留量的测定方法。方法:以二甲基亚砜为溶剂,HP-INNOWAX(PEG-20M)毛细管柱为色谱柱;程序升温;进样口温度200℃,采用氢火焰离子化检测器检测,检测口温度250℃;氮气流速1.5mL·min-1,分流进样,分流比为1∶1;进样量1μL。结果:3种残留有机溶剂正己烷、乙酸乙酯、二氧六环均能达到完全分离,峰面积与浓度均呈良好线性关系(r>0.9999)。最低定量浓度分别为0.027、0.033、0.095μg·mL-1。除2个批号的样品中检出乙酸乙酯含量分别为0.10%与0.15%外,其余各批号均未检出上述3种有机溶剂。结论:该方法简单、灵敏、准确,可同时检测丙酸倍氯米松中的3种有机溶剂的残留量。

OBJECTIVE： To establish a method for the determination of 3 kinds of residual organic solvents in beclometasone dipropionate. METHODS： The residual solvents were separated on HP-INNOWAX capillary column （PEG-20M） with dimethyl sulfoxide as solvent. The programmed temperature was set with injection temperature of 200 ℃. FID detector was applied with injector temperature at 250 ℃ and injection volume of 1 μL. The flow rate of nitrogen was set at 1.5 mL.min^-1 using split inlet. The splitting-ratio was 1 ： 1. RESULTS： Three residual organic solvents consisted of n-hexane, ethyl acetate, dioxane in beclometasone dipropionate were completely separated. The calibration curve of each solvent had good linear relationship （r〉0.999 9）. The minimum quantitative concentrations were 0.027 μg·mL^-1, 0.033 btg.mL-1, 0.095 μg·mL^-1, respectively. The 3 kinds of organic solvents were not found in each batch except 0.10% and 0.15% ethyl acetate was found in 2 batches of samples. CONCLUSIONS： The established method is accurate, sensitive and accurate for the determination of 3 kinds of residual organic solvents in beclometasone dipropionate simultaneously.