静态顶空气相色谱法测定有机残留溶剂二甲基亚砜

Determination of Dimethylsulphoxide as Residual Solvent by Static Headspace Gas Chromatography

建立了高灵敏度、高精确度的静态顶空气相色谱结合氢火焰离子化检测器测定药物辅料中二甲基亚砜残留溶剂的方法。以液体石蜡为溶解溶剂,优化了顶空瓶的液相体积,并对顶空气相色谱的关键实验参数:自动进样时间、顶空加压时间、顶空平衡温度、顶空平衡时间及气相柱温箱升温程序等进行了优化。在最优条件下,确定了方法的检出限和定量限分别为1.0和3.0μg/g。在25～300μg/g浓度范围内,线性回归方程为y=215.49x-828.94,R2=0.9991。应用本方法成功分析了药物包衣材料Kollicoat IR中的残留二甲基亚砜溶剂。

A sensitive,precise static headspace gas chromatography method coupled with flame ionization detection was developed for the analysis of residual dimethyl sulphoxide（DMSO） in drugs.Liquid paraffin oil was used as dilute solvent,liquid volume in the vial and GC parameters such as autosampler injection time,headspace pressurize time,equilibration temperature,equilibration time and oven temperature program were optimized to yield the highest sensitivity.Optimum value of GC parameters such as equilibration temperature,equilibration time,headspace pressurize time,autosampler injection time were 160 ℃,15 min,1.0 min,0.08 min respectively.Limits of detection（LOD） and quantitation（LOQ） were determined to be 1 and 3 μg/g,respectively.Linear regression equation in the range of 25-300 μg/g was y=215.49x-828.94 with R2 of 0.9991.The method was successfully used to analyze residual DMSO in drug coating materials Kollicoat IR.