ICP-AES法测定玻璃类药包材中11种金属元素的浸出量

目的：建立同时测定玻璃类药包材中铝（Al）、钡（Ba）、镉（Cd）、铬（Cr）、铜（Cu）、铁（Fe）、锰（Mn）、铅（Pb）、锑（Sb）、锌（Zn）、铈（Ce）共11种元素的浸出量的分析方法，测定样品，为提高现有标准提供支持和参考。方法： 4%醋酸溶液对玻璃药包材进行浸提，采用电感耦合等离子体发射光谱（ICP-AES）法测定浸提液中11种元素的浓度，高频功率为1.2 kW，等离子体气体流速为10 L·min^-1，分析谱线分别为：394.403（Al）、233.527（Ba）、214.438（Cd）、267.716（Cr）、324.754（Cu）、259.94（Fe）、257.61（Mn）、220.353（Pb）、217.581（Sb）、202.548（Zn）、418.66（Ce）。结果：该方法同时测定Al、Ba、Cd、Cr、Cu、Fe、Mn、Pb、Sb、Zn、Ce，各元素在一定的浓度范围内呈良好的线性关系，线性相关系数为0.999 1~1.000；加样回收率为85.8%~106.0%；精密度试验的RSD为0.4%~1.8%；重复性试验的RSD为0.6%~4.8%；检出限为0.52~75.17ng·mL^-1。测定样品16批，结果测得Al浸出量最高为376.5 ng·mL^-1，Ba浸出量最高为212 ng·mL^-1，其他元素浸出量均较低，大多为未检出。结论：该方法可用于同时测定玻璃类药包材中多种元素的浸出量。结果显示Al浸出量较高，澄清剂氧化铈应用广泛，建议相关标准中增加Al、Ce浸出量的测定方法。

Objective: To establish a method for simultaneous determination of aluminum(Al), barium (Ba), cadmium(Cd), chromium(Cr), copper(Cu), iron(Fe), manganese(Mn), lead(Pb), antimony (Sb), zinc(Zn), cerium(Ce) released from pharmaceutical glass packing material, and to provide reference and support for improving existing standards. Methods: After extracting glass packing material with 4% acetic acid, elements concentrations were simultaneously determined by ICP-AES. Plasma gas flow rate was set at10 L·min^-1 while RF power was 1. 2 kW, and analytical lines of elements were 394. 403(Al), 233. 527 (Ba), 214. 438 (Cd), 267. 716 (Cr), 324. 754 (Cu), 259. 94 (Fe), 257. 61 (Mn),220. 353 (Pb), 217. 581 (Sb), 202. 548 (Zn),and 418. 66 (Ce). Results: The emission intensity of elements showed good linear relationship in a certain concentration ranges as the linear correlation was 0. 999 1-1. 000. The recoveries were 85. 8%-106. 0%. The relative standard deviation of precision was 0. 4%-1. 8%;The relative standard deviation of repeatability was 0. 6%-4. 8%;and the detection limits were 0. 52-75. 17 ng·mL^-1. 16 samples were determined, and the highest concentration of Al was 376. 5 ng·mL^-1,and the highest concentration of Ba was 212 ng·mL^-1, other elements were barely not determined. Conclusion: The method can be used for simultaneous determination of multiple elements released from pharmaceutical glass packing material. The result showed high Al content. In addition,clarifying agent cerium oxide is widely used. Determination of Al and Ce was recommended to be added into the related standard.

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