顶空毛细管气相色谱法测定碘佛醇原料药中的残留溶剂

目的建立测定碘佛醇原料药中甲醇、正丁醇的残留量顶空毛细管气相色谱法。方法以ZB-Wax毛细管柱（30 m×0.32 mm,0.25μm）为色谱柱,水为溶剂,正丙醇为内标,采用顶空进样法测定碘佛醇原料药中甲醇、正丁醇的残留量。结果甲醇、正丁醇质量浓度分别在122.2～366.6μg/mL（r=0.998 3）和128.4～385.2μg/mL（r=0.999 3）范围内呈良好的线性关系,平均加样回收率分别为102.86%（n=9,RSD=1.43%）和96.68%（n=9,RSD=2.69%）,最低检出质量浓度分别为0.66μg/mL和0.04μg/mL。结论该方法简便灵敏,结果准确可靠,能较好地检测碘佛醇原料药中有机溶剂残留量,控制产品质量。

Determination of Residual Solvents in Ioversol Raw Material Drug by Headspace Capillary Gas Chromatography

Objective To establish the headspace capillary gas chromatographic method for the content determination of residual solvents such as methanol and n-butanol in ioversol raw material drug.Methods Methanol and n-butanol in ioversol raw material drug were determined by the headspace gas chromatography with the ZB-WAX capillary column（30 m×0.32 mm,0.25 μm）.Results Methanol and n-butanol showed the linear relation within the concentrations of 122.2-366.6 μg/mL（r=0.998 3） and 128.4-385.2 μg/mL（r=0.999 3）,respectively.The mean recovery rates were 102.86%（n=9,RSD=1.43%）and 96.68%（n=9,RSD=2.69%）,respec-tively.The detection limits were 0.66 μg/mL and 0.04 μg/mL.Conclusions This established method is simple,sensitive,accurate and reliable for the content determination of residual solvents in ioversol raw material drug and the quality control of this product.