气相色谱法测定药用辅料聚西托醇1000中的残留杂质

Determination of residual impurities in pharmaceutical excipient cetomacrogol 1000 by gas chromatography

建立气相色谱法测定聚西托醇1000中残留的环氧乙烷、1,4-二氧六环、乙二醇、二甘醇和三甘醇等杂质,为聚西托醇1000生产质量控制提供参考。采用DB-1色谱柱检测环氧乙烷和1,4-二氧六环,顶空进样,进样口温度150℃,检测器温度250℃,顶空平衡温度70℃,平衡时间45 min。采用VF-17MS色谱柱检测乙二醇、二甘醇和三甘醇,液体进样,进样口温度270℃,检测器温度290℃。实验结果显示,环氧乙烷和1,4-二氧六环在各加样量范围内线性良好(r>0.999),精密度RSD小于8.0%,平均回收率分别为90.6%和101.2%;乙二醇、二甘醇和三甘醇在3~60μg/mL内线性关系良好(r>0.999),精密度RSD小于3.0%,回收率均在96%~103%。本研究所建立的方法具有良好的专属性、线性、精密度和回收率,能够有效检测聚西托醇1000中多组分极微量杂质。

For the quality control of cetomacrogol 1000,a gas chromatographic method for the determination of residual impurities in cetomacrogol 1000,such as ethylene oxide,1,4-dioxane,ethylene glycol,diethylene glycol and triethylene glycol,was established and validated.The DB-1 column with headspace injection was used to detect ethylene oxide and 1,4-dioxane with the inlet temperature of 150°C,the FID temperature of 250°C,the headspace equilibration temperature of 70°C and the equilibration time of 45 min.The VF-17MS column with liquid injection was used to detect ethylene glycol,diethylene glycol and triethylene glycol with the inlet temperature of 270°C,and the FID temperature of 290°C.The results showed that ethylene oxide and 1,4-dioxane have a good linearity within their specified addition amount ranges(r>0.999),with the RSD of precision of below 8.0%and the average recovery rates of 90.6%and 101.2%;and that ethylene glycol,diethylene glycol and triethylene glycol also have a good linearity between 3‒60μg/mL(r>0.999),with the RSD of precision of below 3.0%,and the recovery rates of 96%~103%.The method established in this study has good specificity,linearity,precision and recovery rate,which can effectively detect the multi-component and trace impurities.