ICP-MS 法测定富马酸沃诺拉赞原料药中镍钯的残留量

Determination of Residual Nickel and Palladium in Vonoprazan Fumarate by ICP-MS

  • 摘要: 本文建立了一种电感耦合等离子体质谱仪测定富马酸沃诺拉赞原料药中催化剂镍、钯残留的方法。以硝酸 -高氯酸为混合消解液,采用湿法消解对富马酸沃诺拉赞原料药进行前处理,用 ICP-MS 法对其中镍、钯含量进行定量分析。通过配制钯、镍元素标准溶液,验证标准曲线和相关系数,确定该方法相关系数均在 0.9999 以上。根据该方法,镍方法检出限为 3.03 μg·kg-1,钯方法检出限为 8.60 μg·kg-1,两种元素精密度 RSD 在 2.00% 以内,回收率在96.0%~105.7% 之间。所建立的方法精密度、重复性结果良好,准确度高,可用于富马酸沃诺拉赞原料药中镍、钯残留的检测。

     

    Abstract: A method for the determination of nickel and palladium residues in Vonoprazan fumarate by inductively coupled plasma mass spectrometry (ICP-MS) has been developed. Vonoprazan fumarate was pretreated by wet digestion with nitric acid, perchloric acid as the mixed digestion solution, detected the content of nickel and palladium by ICP MS. The standard curve and correlation coefficient were verified through palladium and nickel standard solution, the correlation coefficient of this method was above 0.9999, the detection limit of nickel method was 3.03 μg·kg-1, the detection limit of palladium method was 8.60 μg·kg-1, the RSD of the two elements was within 2.00%, and the recovery was between 96.0% and 105.7%. This method has high precision, repeatability and accuracy, this method can be used for the determination of nickel and palladium residues in Vonoprazan fumarate.

     

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