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目的建立微波消解-电感耦合等离子体原子发射光谱(inductively coupled plasma atomic emission spectrometry,ICP-AES)法检测屋尘螨变应原制品中铝含量,并进行验证。方法采用微波消解法对样品进行消解处理后,用ICPAES法测定样品中的铝含量,并对建立的方法进行线性范围、精密度、准确性验证,确定最低检出限和最低定量限;用建立的方法检测2批次屋尘螨变应原制剂中的铝含量。结果该方法铝元素浓度在0~0.30μg/ml范围内与分析线的响应值具有良好的线性关系(r=0.999 552);0.10μg/ml标准品溶液连续进样11次,铝含量平均值为0.100 2μg/ml,相对标准偏差(RSD)为1.2%;6份样品溶液的铝含量平均值为10.90μg/ml,RSD为1.4%;3份样品溶液的平均加标回收率为95.5%,RSD为4.9%;该方法最低检出限为0.008 5μg/ml,最低定量限为0.028μg/ml。2批次共5份屋尘螨变应原制剂样品中铝含量测定结果均符合该企业注册标准中铝含量标准要求。结论微波消解法对样品消解完全,采用微波消解-ICP-AES法可以对屋尘螨变应原制品中的铝含量进行准确定量,该方法操作简便,灵敏度、精密度、准确度良好。
Objective To establish and verify the aluminum content in allergens of house dust mite by inductively coupled plasma atomic emission spectrometry (ICP-AES). Methods The sample was digested by microwave digestion method, the content of aluminum in the sample was determined by ICPAES method, and the linear range, precision and accuracy of the established method were validated to determine the minimum detection limit and the minimum quantitative limit; Method to detect aluminum content in two batches of house dust mite allergen preparations. Results The concentration of aluminum in the range of 0 ~ 0.30μg / ml had a good linear relationship with the analytical line response (r = 0.999 552). The standard solution of 0.10μg / ml was injected 11 times continuously and the average content of aluminum 0.100 2μg / ml with relative standard deviation (RSD) of 1.2%. The average content of aluminum in 6 samples was 10.90μg / ml and the RSD was 1.4%. The average recoveries of three samples were 95.5% RSD was 4.9%. The detection limit was 0.008 5μg / ml and the lowest limit of quantification was 0.028μg / ml. 2 batches of a total of 5 house dust mite allergen preparations aluminum content determination results are in line with the registration standards of the enterprise aluminum content standards. Conclusion The sample digestion with microwave digestion is complete. The content of aluminum in house dust mite allergen can be accurately quantified by microwave digestion-ICP-AES. The method is simple, sensitive, precise and accurate.