电感耦合等离子体质谱法测定甘油(供注射用)中7种元素杂质含量

Determination of 7 Elemental Impurities in Glycerol for Injection by ICP-MS

目的:建立用电感耦合等离子体质谱(ICP-MS)测定甘油(供注射用)中镉、铅、砷、汞、钴、钒、镍7种元素杂质含量的方法。方法:微波消解法处理样品采用ICP-MS法测定射频功率1500 W,采用碰撞模式,碰撞气为氦气,载气为氩气,载气流速0.7 L·min-1,等离子体气体流速15.0 L·min-1,泵速0.3r·s-1。结果:7种元素线性关系良好(r>0.9990);加样回收率为94.2%~107.0%(n=9);检测限为0.0002~0.006μg·g-1,定量限为0.05~0.5μg·g-1。结论:本方法准确可靠、灵敏简便,可用于甘油(供注射用)中多种元素杂质的质量研究同时为测定同类药用辅料中此7种元素杂质提供参考。

Objective:To establish a method for the determination of 7 elemental impurities(Cd,Pb,As,Hg,Co,V and Ni)in glycerol for injection by inductively coupled plasma-mass spectrometry(ICP-MS).Methods:Microwave digestion was adopted for the sample pretreatment.An ICP-MS method was established with following conditions:the RF power was 1500 W,the collision gas was He,the carrier gas was argon,the flow rate of the carrier gas was 0.7 L·min-1,the flow rate of the plasma gas was15.0 L·min-1,and the pump speed was 0.3 r·s-1.Results:The linearities of the 7 elemental impurities were good(r>0.9990);the average recoveries were from 94.2%to 107.0%(n=9)the limits of detection were from 0.0002 to 0.006μg·g-1 and the limits of quantitation were from 0.05 to 0.5μg·g-1.Conclusion:The method is accurate,sensitive and convenient,and can support the determination of 7 elements in glycerol for injection,which provides reference and method for the further research of other pharmaceutical excipients.