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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(30 m×0.32 mm,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0.997 9~0.999 5之间;3个水平的回收率分别在81%~108%之间,各组分检出限在0.049 7~0.499μg·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 headspace gas chromatographic method for the determination of seven residual solvents in vidarabine monophosphate drug substance. Methods: DB-624 capillary column (30 m × 0.32 mm, 1.8 μm) was used as the chromatographic column. Methanol, ethanol, acetone, acetonitrile, methylene chloride and ethyl acetate Ester and pyridine content. Results: The separation of methanol, ethanol, acetone, acetonitrile, methylene chloride, ethyl acetate and pyridine was good. The concentration of seven organic solvents showed a good linear relationship with the concentration in the concentration range studied. The correlation coefficient was 0.997 9 ~ 0.999 5; the recoveries of the three levels were between 81% and 108%, and the detection limits of each component were between 0.049 7 and 0.499 μg · mL -1. Conclusion: This method is accurate and sensitive and can be used for the determination of residual solvents in the raw drug of glyphosate monophosphate.