顶空-气相色谱法测定硫酸羟氯喹中环氧乙烷残留量的方法学研究

Methodology Study of Determination of Potential Genotoxic Impurity Ethylene Oxide Residue in Hydroxychloroquine Sulfate by Headspace-Gas Chromatography

采用顶空-气相色谱法测定硫酸羟氯喹潜在基因毒性杂质环氧乙烷的残留量。在选用的色谱条件下,硫酸羟氯喹供试品溶液中的杂质峰及空白溶液对检测均无干扰,分离效果良好,专属性高;检测限与定量限的质量浓度皆远低于限度,定量限质量浓度下6份样品的峰面积相对标准偏差(RSD)小于10.0%,保留时间的RSD小于2.0%,表明方法灵敏度良好;在1.6033~21.3780 mg/L范围内,质量浓度与峰面积成线性关系(r=0.9995)。该方法色谱条件简便,检测快速,结果准确、稳定,耐用性优异,可用于测定硫酸羟氯喹潜在基因毒性杂质环氧乙烷的残留量。

The residual amount of ethylene oxide,a potentially genotoxic impurity of hydroxychloroquine sulfate,was determined by headspace-gas chromatography.Under the selected chromatographic conditions,the impurity peaks in the hydroxychloroquine sulfate test solution and the blank solution had no interference to the detection,with good separation effect and high specificity.The detection limit and the quantification limit were far lower than the specified concentration.The relative standard deviation(RSD)of peak area of the 6 samples at the limit of quantification concentration was less than 10.0%,and the RSD of retention time was less than 2.0%,indicating that the sensitivity of the method was good.In the range of 1.6033-21.3780 mg/L,there was a linear relationship between the mass concentration and the peak area(r=0.9995).The method has the advantages of simple chromatographic conditions,rapid detection,accurate and stable results and excellent durability,and it can be used to determine the residual amount of ethylene oxide in hydroxychloroquine sulfate.