ICP-OES法测定13价肺炎球菌结合疫苗中的铝含量

目的:建立电感耦合等离子原子发射光谱(inductively coupled plasma optical emission spectrometry,ICP-OES)的方法检测13价肺炎球菌结合疫苗中的铝含量。方法:采用ICP-OES法测定样品中的铝含量,比较微波消解法和0.1 mol·L^-1盐酸溶液直接处理方法。结果:在本文条件下,0.1 mol·L^-1盐酸溶液处理样品与微波消解法处理样品后用ICP-OES法测定铝含量,结果无统计学意义,选择0.1 mol·L^-1盐酸处理样品。在此条件下,铝元素质量浓度在1~20 μg·mL^-1范围内,与响应值具有良好的线性关系(r=0.9999);重复性RSD均低于4%;铝含量回收率在90%~110%;该方法的检出限为0.015 μg·mL^-1,定量限为0.050 μg·mL^-1;专属性考察结果显示,0.04%氯化钠0.1 mol·L^-1盐酸和0.1 mol·L^-1氯化锂0.1 mol·L^-1盐酸均不影响铝含量的检测;溶液稳定性研究结果证明,0.1 mol·L^-1盐酸稀释的样品溶液在室温放置5d内稳定性良好。3批次13价肺炎球菌结合疫苗中铝含量检测值均符合该企业注册标准中铝含量标准。结论:所建立的ICP-OES法可用于对13价肺炎球菌结合疫苗中的铝含量进行准确定量,检测方法操作简便,灵敏度、精密度、准确度良好。

Objective: To establish an inductively coupled plasma optical emission spectrometry (ICP-OES)method for the determination of the aluminum content in 13-valent pneumococcal conjugated vaccine.Methods:ICP-OES was adopted to determine the aluminum content in 13-valent pneumococcal conjugated vaccine,and the treatment of microwave digestion and the direct treatment with 0.1 mol·L^-1 hydrochloric acid were compared.Results:The results of aluminum contents were no statistically significant between the microwave digestion group and the 0.1 mol·L^-1hydrochloric acid group for 13-valentpneumococcal conjugate vaccine,so 0.1 mol·L^-1 hydrochloric acid treatment was chosen.Under these conditions in this study,the linear relationship in the range of 1-20 μg·mL^-1 aluminum content was good,r=0.999 9.The RSDs of repeatability were lower than 4%.The recoveries were in the range of 90%-110%.The specificity results showed that 0.04% NaCl 0.1 mol·L^-1hydrochloric acid and 0.1 mol·L^-1 LiCl 0.1 mol·L^-1 hydrochloric acid had no influence on the detection of aluminum.The stability results showed that the aluminum content was stable in 0.1 mol·L^-1 hydrochloric acid treated samples placed at room temperature for 5 days.The minimum detection limit of the method was 0.015 μg·mL^-1,while the minimum quantitation limit was 0.050 μg·mL^-1.The determination results of three batches met the license requirements.Conclusion: The aluminum contents in 13-valent pneumococcal conjugated vaccine were accurately determined by ICP-OES.This method was precise,accurate and sensitive.