电感耦合等离子体质谱法测定马来酸氟伏沙明片元素杂质

Determination of the Elemental Impurities in Fluvoxamine-Maleate Tablets by ICP-MS

目的采用电感耦合等离子体质谱(ICP-MS)法测定马来酸氟伏沙明片中1类(镉Cd、砷As、铅Pb、汞Hg)和2A类(钴Co、钒V、镍Ni)元素杂质,为评估和控制产品中的元素杂质提供支持。方法马来酸氟伏沙明片采用加硝酸微波消解的方式处理,采用45Sc、89Y作为内标,雾化气流速为1.0 L/min,冷却气流速为14.0 L/min,辅助气流速为0.8 L/min。结果7种待测元素在LOD~400μg/L的浓度范围内线性关系良好,相关系数r≥0.999,检测限在0.026~0.246μg/L,各元素的回收率在90.8%~104.4%,重复性及中间精密度的相对标准偏差(RSD)分别在8.7%、7.3%以内。结论方法重复性好、灵敏度高,可以用于测定马来酸氟伏沙明片中7种元素杂质。

Objective To determine the type 1(Cd,As,Pb,Hg)and type 2 A(Co,V,Ni)element impurities in fluvoxamine maleate tablets by ICP-MS,and to provide support for evaluating and controlling elemental impurities in products.Methods Fluvoxamine maleate tablets were processed by microwave digestion with nitric acid.45Sc and 89Y were used as internal standards.The atomizing gas flow rate was 1.0 L/min,the cooling gas flow rate was 14.0 L/min,and the auxiliary gas flow rate was 0.8.L/min.Results The 7 analyte elements had a good linear relationship within the concentration range of LOD-400μg/L,the correlation coefficient r≥0.999,the limit of detection was between 0.026-0.246μg/L,and the recovery rate of each element was between 90.8%-104.4% The RSD of repeatability and intermediate precision were within 8.7% and 7.3% respectively.Conclusion The method has good reproducibility and high sensitivity,and can be used to determine 7 element impurities in fluvoxamine maleate tablets.