ICP-MS直接进样测定小儿钠钾镁钙葡萄糖注射液中11种元素杂质含量

Content determination of 11 element impurities by ICP-MS through direct injection technique in sodium potassium magnesium calcium and glucose injection for children

目的:建立ICP-MS直接进样法测定小儿钠钾镁钙葡萄糖注射液中锂、钒、铁、钴、镍、铜、砷、镉、锑、汞、铅11种元素杂质含量。方法:采用ICP-MS进行测定,测定模式为He模式,等离子体模式为耐高盐进样HMI-8,采样深度10.0 mm,射频功率:1600 W,雾化气流量0.67 L·min-1,稀释气流量0.26 L·min-1,辅助气流量0.9 L·min-1,等离子气流量15.0 L·min-1,蠕动泵转速0.10 rps,雾化室温度2.0℃。结果:11种元素杂质线性相关系数r均大于0.9990;检测限与定量限均小于限度浓度的10%;加样回收率在83.42%~111.62%范围内;重复性RSD≤4.46%;中间精密度RSD≤5.19%。3批样品中11种元素杂质含量均符合限度要求。结论:建立的小儿钠钾镁钙葡萄糖注射液中11种元素杂质的测定方法灵敏度高,样品直接进样基质干扰小,适用于小儿钠钾镁钙葡萄糖注射液中元素杂质的控制研究。

Objective:To establish an inductively coupled plasma mass spectrometry(ICP-MS)method with direct injection technique to detect 11 element impurities(Li,V,Fe,Co,Ni,Cu,As,Cd,Sb,Hg,Pb)in sodium potassium magnesium calcium and glucose injection for children.Methods:ICP-MS was used for determination with He mode.The plasma mode was HMI-8,a halophilic sampling system.The sampling depth was 10.0 mm.The power of radio frequency was 1600 W.The nebulizer gas flow was 0.67 L·min-1.The dilution gas flow was 0.26 L·min-1.The auxiliary gas flow was 0.9 L·min-1 and the plasma gas flow was 15.0 L·min-1.The speed of nebulizer pump was 0.10 rps and the temperature of atomizer chamber was 2.0℃.Results:Regression coefficients of the standard curve of the 11 elements impurities were all more than 0.9990.The limit of detection and quantitation were all less than 10%of the limit concentration.The recovery rate was within the range of 83.42%–111.62%.The RSD of repeatability and intermediate precision was less than or equal to 4.46%and 5.19%respectively.The contents of 11 element impurities in 3 batches of samples all met the limit requirements.Conclusion:The established method in our study was highly sensitive and had little groundmass interference with direct injection technique,which were suitable for the control of element impurities in sodium potassium magnesium calcium and glucose injection for children.