目的: 根据ICH Q3D最新要求,建立同时测定注射用头孢美唑钠中10种元素杂质的方法。方法: 样品经直接溶解并稀释后采用电感耦合等离子质谱分析,以硒(Se)、锗(Ge)、碲(Te)、镥(Lu)为内标,等离子功率1 550 W,载气流量1.09 L·min-1。结果: 10种元素线性均良好(r均>0.999),检测限为0.000 2~0.059 ng·mL-1,各浓度点平均回收率为90%~110%(n=3),重复性RSD为4%~10%(n=6)。5家企业12批样品中有3批测得镍(Ni)(0.1 μg·mL-1),其中1批测得锂(Li)(0.1 μg·mL-1),不同厂家的注射用头孢美唑钠中10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,可用于注射用头孢美唑钠中元素杂质的质量控制。
Objective: To develop a method for simultaneous determination of 10 elemental impurities in cefmetazole sodium for injection according to the latest requirement of ICH Q3D. Methods: Samples were analyzed after direct dissolved and dilution by inductively coupled plasma mass spectroscopy (ICP-MS), with selenium (Se), germanium (Ge), tellurium (Te), and lutetium (Lu)as internal standards. RF power was set at 1 550 W and carrier gas was set at 1.09 L·min-1. Results: The linear relationship for all elemental impurities were good(r＞0.999), with a detection limit of 0.000 2-0.059 ng·mL-1. The average recovery rate at each concentration point was 90%~110% (n=3), and the RSD were 4%-10% (n=6). Nickel (Ni) were detected at 0.1 μg·mL-1 in 3 out of 12 batches of samples from five companies, and lithium (Li) was detected at 0.1 μg·mL-1 in 1 batche. The contents of 10 elemental impurities in cefmetazole sodium for injection from different manufacturers comply with ICH requirement. Conclusions: The established method was simple, rapid, sensitive, accurate and can be used for the quality control of elemental impurities in cefmetazole sodium for injection.
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