ICP-OES法测定药用卤化丁基橡胶塞中7种金属元素的浸出量

目的：建立ICP-OES法检测药用卤化丁基橡胶塞中Al、Ca、Mg、Fe、Si、Ti、Zn 7种金属元素，并对10批样品中7种金属元素的浸出量进行测定。方法：高频功率为1 150 W，等离子体气流速10 L·min^-1，分析谱线：308.2（Al）、396.8（Ca）、280.2（Mg）、238.2（Fe）、212.4（Si）、336.1（Ti）、206.2（Zn）。结果：Al、Ca、Mg、Fe、Si、Ti、Zn 7种元素在0.05～5 μg·mL^-1质量浓度范围内呈良好的线性关系，线性相关系数为0.999 5～0.999 9；加样回收率为93.8%～107.2%；精密度试验的RSD为0.28%～1.6%；稳定性试验的RSD为1.2%～3.6%；重复性试验的RSD为0.34%～1.9%；检测下限为0.15～3.51 ng·mL^-1。10批样品中，部分样品中检出微量Ca、Mg、Si、Zn，Al和Ti检出量较低，Fe元素均未检出。结论：经方法学验证，本法可用于测定药用卤化丁基橡胶塞中7种金属元素的浸出量。根据样品测定结果，建议相关标准中增加Ca、Mg、Si、Zn浸出量的监测。

Objective: To establish an ICP-OES method for determination of 7 metal elements,including Al,Ca,Mg,Fe,S,Ti and Zn,in pharmaceutical halogenated butyl rubber stopper,and to determination the leaching amounts of 7 metal elements in 10 batches of samples. Methods: The plasma gas flow rate was set at 10 L·min^-1 while RF powers was 1 150 W,and analytical lines of element were 308.2 nm(Al),396.8 nm(Ca),280.2 nm(Mg),238.2 nm(Fe),212.4 nm(Si),336.1 nm(Ti),206.2 nm(Zn). Results: This method could measure Al,Ca,Mg,Fe,S,Ti and Zn at the same time,and each element showed a good linear relationship within the range of 0.05-5 μg·mL^-1,the linear correlation coefficient were 0.999 5-0.999 9;the recovery rate were 93.8%-107.2%;the relative standard deviation of precision was 0.28%-1.6%;the relative standard deviation of stability was 1.2%-3.6%;the relative standard deviation of repeatability was 0.34%~1.9%;and the detection limits were 0.15- 3.51 ng·mL^-1. In the 10 batches of samples,Ca,Mg,Si,Zn and trace of Al and Ti were detected,while Fe was not detected. Conclusion: The method can be used to determine the leaching amount of 7 elements in halogenated butyl rubber stopper.According to the results of sample measurement,it is suggested to enhance the monitoring of Ca,Mg,Si and Zn leaching in the relevant standards.

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