大口径毛细管气相色谱检查药物中残留溶剂的方法研究

 以药物合成中常用的 16种有机溶剂为研究对象 ,建立了用大口径毛细管柱检查残留有机溶剂的气相色谱法 ,并考察了不同极性的色谱柱及不同提取溶剂对分离与检测的影响。实验表明 ,根据原料药合成中可能存在的残留溶剂 ,选用适当的提取溶剂 ,采用大口径毛细管气相色谱法检查 ,可获得较满意的结果。

Study on Gas Chromatographic Method for the Evaluation of Residual Solvents by Using Wide Bore Open Tubular Columns

A GC method using wide bore open tubular columns was developed to evaluate residual organic solvents. Sixteen organic solvents commonly used for pharmaceutical synthesis were analysed.The effects of different polarity columns and extraction solvents on the assay of residual solvents were studied in this work. It showed that most solvents can be well separated from each other on non polar or less polar wide bore columns. Extraction solvents differed in their extraction recovery and peak shape. Satisfactory results can be obtained when the proposed method was employed and a suitable extraction solvent was selected.The procedures summarized in this paper can be used as a guidance for the evaluation of residual organic solvents in bulk pharmaceuticals.