葡萄糖酸钙注射液中24种元素杂质测定方法的建立

A method for the determination of 24 elemental impurities in calcium gluconate injection

目的:根据ICH Q3D最新要求,建立同时测定葡萄糖酸钙注射液中24种元素杂质的方法。方法:样品经直接稀释后采用电感耦合等离子质谱分析,以Sc、In、Bi为内标,等离子功率1500 W,载气流量1.05L·min-1。结果:24种元素线性均良好(r均大于0.999),检测下限为0.0002~0.005 ng·mL-1,各浓度点平均回收率为98.5%~123.8%(n=3),重复性为2.6%~6.0%(n=6),中间精密度为3.4%~7.5%(n=12)。不同厂家的葡萄糖酸钙注射液中24种元素杂质含量均符合ICH规定。结论:本文应用的方法简单快速,灵敏度高,准确性好,可用于葡萄糖酸钙注射液中元素杂质的质量控制。

Objective:To develop a method for simultaneous determination of 24 elemental impurities in calcium gluconate injection according to the latest requirement of ICH Q3 D.Methods:Samples were analyzed after direct dilution by inductively coupled plasma mass spectroscopy(ICP-MS)with Sc,In and Bi as internal standard.RF power was set at 1500 W and carrier gas was set at 1.05 L·min-1.Results:The linear relationship for all elemental impurities was good(r>0.999).Detection limits were between 0.0002-0.005 ng·mL-1.The recoveries were between 98.5%-123.8%(n=3).The repeatability and intermediate precision were between 2.6%~6.0%(n=6)and 3.4%-7.5%(n=12),respectively.The contents of 24 elemental impurities in calcium gluconate injection from different manufacturers comply with ICH requirement.Conclusion:The established method is simple,rapid,sensitive,accurate and applicable for the elemental impurity control of calcium gluconate injection.