离子色谱法测定依达拉奉注射液中亚硫酸盐

Determination of sulfite ion of edaravone injection by ion chromatography

建立测定依达拉奉注射液中亚硫酸根离子含量的离子色谱法。采用IonPac AS11-HC阴离子分析柱(250mm×4.6 mm,7.5μm),柱温为25℃,以15 mmol/L氢氧化钾溶液作为淋洗液,流量为1.0 mL/min,检测器为电导检测器,检测器温度30℃,抑制器为自动再生抑制模式,抑制电流40 mA,进样体积为25μL,用离子色谱法测定亚硫酸盐,硫酸根离子质量浓度在0.1~200μg/mL范围内与色谱峰面积线性关系良好,相关系数为0.9998。该方法检出限为0.027μg/mL,定量限为0.072μg/mL。亚硫酸根离子在水溶液中8 h内稳定。样品加标回收率为98.5%~100.6%,相对标准偏差为0.7%(n=9)。该方法操作简单,专属性强,灵敏度高,重复性好,可用于依达拉奉注射液中亚硫酸盐含量的测定。

An HPLC method was establishd for the determination of sulfite ion of edaravone injection by ion chromatography.The chromatographic colum was IonPac AS11-HC column(250 mm×4.6 mm,7.5μm),the colum temperature was 25℃,the eluent was 15 mmol/L potassium hydroxide solution with the flow rate of 1.0 mL/min,the detector was a conductivity detector,the detector temperature was 30℃,the suppressor was in automatic regeneration suppression mode.The suppression current was 40 mA,and the injection volume was 25μL.Determination of Sulfite by ion chromatography,mass concentration of sulfite ion had linear relationship in the range of 0.1 to 200μg/mL with the corelation coefficient of 0.9998.The detection limit was 0.027μg/mL,and the limit of quantification was 0.072μg/mL.Sulfurous acid ion was stable in aqueous solution for 8 h.The recovery range was 98.5%to 100.6%with the relative standard deviation of 0.7%(n=9).The method has the advantages of simple operation,strong specificity,high sensitivity and good repeatability,which can be used for the determination of sulfite in edaravone injection.