微波消解-电感耦合等离子体质谱法测定依度沙班原料药中36种金属元素

Determination of 36 metal elements in edoxaban by microwave digestion-ICP-MS

建立微波消解-电感耦合等离子体质谱法测定依度沙班原料药中36种金属元素的方法。采用微波消解法对样品进行前处理,以HNO_(3)和H_(2)O_(2)作为消解体系,以Rh,Re作为内标,用电感耦合等离子体质谱法进行测定。各元素的质量浓度在0〜50μg/L范围内与信号强度的线性关系良好,相关系数均大于0.9995,检出限为0.001-0.968μg/L。测定结果的相对标准偏差为0.07%〜1.40%(n=6),样品加标回收率为94.7%〜106.0%。该方法操作简便快速、灵敏可靠,适用于依度沙班原料药中金属元素的测定。

A method for the determination of 36 metal elements in edoxaban by microwave digestion-inductively coupled plasma mass spectrometry(ICP-MS)was established.The sample was pretreated by microwave digestion,HNO_(3)and H_(2)O_(2)were used as digestion system,Rh and Re were used as internal standards,and ICP-MS was used for determination.The mass concentration of each element had good linear relationship with the signal intensity in the range of 0-50μg/L,the correlation coefficients were more than 0.9995,the detection limits were 0.001-0.968μg/L.The relative standard deviations of the determination results were 0.07%-1.40%(n=6),and the recoveries were 94.7%-106.0%.The method is simple,rapid,sensitive and reliable,which is suitable for the determination of metal elements in edoxaban.