目的: 建立测定单磷酸阿糖腺苷原料药中7种残留溶剂的顶空气相色谱法。方法: 使用DB-624毛细管柱(30m×0.32mm,1.8μm)为色谱柱,以水为溶剂,测定单磷酸阿糖腺苷原料中甲醇、乙醇、丙酮、乙腈、二氯甲烷、乙酸乙酯和吡啶的含量。结果: 甲醇、乙醇、丙酮、乙腈、二氯甲烷、乙酸乙酯和吡啶分离度好,在所考察的浓度范围内7种有机溶剂的峰面积与浓度呈良好的线性关系,相关系数在0.9979~0.9995之间;3个水平的回收率分别在81%~108%之间,各组分检出限在0.0497~0.499μg·mL^-1之间。结论: 此方法准确、灵敏,可用于单磷酸阿糖腺苷原料药中残留溶剂的测定。

OBJECTIVE To establish a method for determining seven residual solvents in vidarabine monophosphate by headspace gas chromatography.METHODS Residual solvents including methanol, ethanol, acetone, acetonitrile, dichloromethane, ethyl acetate and pyridine in vidarabine monophosphate were quantitatively determined on a DB-624 column (30 m×0.32 mm,1.8 μm), with water as solvent.RESULTS Seven residual solvents were completely separated. The method had a good linear relationship in proper concentration range and regression coefficients were between 0.997 9 and 0.999 5. Three levels of recovery were in range of 81%-108%. Detectable limit was 0.049 7-0.499 μg·mL^-1.CONCLUSION This method is accurate and sensitive, which can be used for determination of residual solvents in vidarabine monophosphate.