PTV—GC测定药品中环氧氯丙烷溶剂残留的研究

[目的]建立药品中环氧氯丙烷有机残留大体积进样、程序升温气化、气相色谱测定方法。[方法]取一定量样品，加入二硫化碳溶液萃取后大体积进样（30μl），经程序升温气化进样-气相色谱测定，进行定量测定。[结果]在上述条件下．该方法的检出限为0．00015％．日内精密度为6．28％～7．81％，日间精密度为7．97％～8．94％，回收率为89．3％～96．7％，线性范围0．145-2．360μg／ml，相关系数0．9975。[结论]该方法操作简单、灵敏度高，可以用于药品中环氧氯丙烷残留的测定。

Determination of Residual Epichlorohydrin in Drug by PTV-GC

[Objective]To establish a PTV-GC（programmed temperature vaporization-gas chromatography） method for the determination of residual epichlorohydrin in drug. [Methods]Epichlorohydrin in drug was extracted by carbon disulfide. The extract was analyzed by GC with a programmable temperature vaporizer in large volume injection（30 μl）. [Results]The range of calibration curve was 0. 145-2. 360 μg/ml, with the determination limit of 0. 000 15 %. The recovery of the method was between 89.3 % and 96.7 %, the precision RSD 〈 100%. [Conclusion] The method is easy to operate and with high sensitiveness. It is suitable for determination of residual epichlorohydrin in drug.