屋尘螨变应原制品中铝含量微波消解-电感耦合等离子体原子发射光谱检测方法的建立

Development and verification of microwave digestion-inductively coupled plasma atomic emission spectrometry for aluminum content in house dust mite allergen products

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 develop and verify the microwave digestion-inductively coupled plasma atomic emission spectrometry（ICP-AES）for quantitative determination of aluminum content in house dust mite allergen products. Methods The samples were digested by microwave digestion,and determined for aluminum content by ICP-AES. The developed method was verified for linear range,precision and accuracy,and determined for minimum detection and quantitation limits. The aluminum contents in two batches of house dust mite allergen products were determined by the developed method. Results The developed method showed good linearity within an aluminum concentration range of 0 ~ 0. 30 μg / ml（r = 0. 999 552）. The standard solution at a concentration of 0. 10 μg / ml was determined for 11 times,and the result showed a mean aluminum content of 0. 100 2 μg / ml,with a RSD of 1. 2%. The mean aluminum content in six samples was 10. 90 μg / ml,with a RSD of 1. 4%. However,the mean spike recovery rate of three samples was 95. 5%,with a RSD of 4. 9%. The minimum detection limit of the method was 0. 008 5 μg / ml,while the minimum quantitation limit was 0. 028 μg / ml. The determination results of five samples from two batches of house dust mite allergen products met the requirements for license. Conclusion The samples were completely digested by microwave digestion method. The aluminum contents in house dust mite allergen products were accurately determined by microwave digestion-ICP-AES. The method was simple,sensitive and accurate.