微波消解-电感耦合等离子体质谱法测定阿普米司特片中7种杂质元素

Determination of 7 elemental impurities in Apremilast Tablets by microwave digestion-inductively coupled plasma mass spectrometry

建立微波消解-电感耦合等离子体质谱法同时测定阿普米司特片中砷、镉、汞、铅、钴、镍、钒7种杂质元素的分析方法。样品以硝酸-氢氟酸体系为消解溶剂,采用微波消解,以铬、锗、铑、铼为内标,采用电感耦合等离子体质谱法进行测定。7种元素的质量浓度在一定范围内与质谱响应值线性相关性良好(r≥0.999),检出限均小于0.2ng/mL,定量限均小于0.6 ng/mL,远低于阿普米司特片中对应元素的控制限量。样品测定值相对标准偏差为1.5%~2.8%(n=6),样品加标平均回收率均为97.5%~100.7%。该方法操作简单快速,灵敏度较高,适用于阿普米司特片中7种杂质元素的同时检测。

A method was established for the simultaneous determination of 7 elemental impurities including As,Cd,Hg,Pb,Co,Ni and V in Apremilast tablets by microwave digestion-inductively coupled plasma mass spectrometry.The samples were pretreated by microwave digestion with HNO3 and HF as digestion system,and determined by inductively coupled plasma mass spectrometry(ICP-MS) with Cr,Ge,Rh and Re as internal standards.The linear relationships of 7elemental impurities was good within their respective detection mass concentration ranges(r≥0.999).The detection limits were all below 0.2 ng/mL,and the quantification limits were all below 0.6 ng/mL,which were lower than control limits in Apremilast tablets.The relative standard deviations of detection results were 1.5%-2.8%(n=6),and the average recoveries of accuracy were 97.5%-100.7%.The method is simple,rapid,and sensitive which is suitable for the determination of elemental impurities in Apremilast tablets.