葡萄糖酸钙注射液中24种元素杂质测定方法的建立

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1 500 W，载气流量1.05 L·min^-1。结果： 24种元素线性均良好（r均大于0.999），检测下限为0.000 2~0.005 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 Q3D. 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 1 500 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 0.000 2-0.005 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.

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