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目的建立电感耦合等离子体质谱(inductively coupled plasma-mass spectrometry,ICP-MS)法测定螨变应原注射液中的铝含量,并进行验证及初步应用。方法样品经微波消解后,采用ICP-MS法测定其中的铝含量。确定ICPMS法的线性范围及最低检出限,并进行精密性、重现性、准确性验证。用建立的ICP-MS法检测2批螨变应原注射液样品的铝含量;分别采用建立的ICP-MS法和该制品进口检验标准中的比色法检测5批螨变应原注射液样品的铝含量。结果建立的ICP-MS法的线性范围为0~100 ng/ml,r=0.999 9;最低检出限为0.111 ng/ml;该方法重复检测6次10 ng/ml标准溶液铝含量的相对标准偏差(relative standard deviation,RSD)为2.56%;检测6份样品铝含量的RSD值为1.13%;检测9份样品铝含量的总平均加标回收率为95.7%,RSD值为1.37%。该方法检测2批螨变应原注射液样品中的铝含量,结果均符合其标准要求;建立的ICP-MS法与比色法检测5批螨变应原注射液样品中铝含量的结果基本一致。结论建立了ICP-MS法检测螨变应原注射液中的铝含量,该方法操作简便、快速,精密性、重现性、准确性良好,为螨变应原注射液质量标准的提高奠定了基础。
Objective To establish an inductively coupled plasma-mass spectrometry (ICP-MS) method for the determination of aluminum in mite allergen injection, and to verify and preliminary apply it. Method After microwave digestion, the content of aluminum in the sample was determined by ICP-MS. ICPMS method to determine the linear range and minimum detection limit, and precision, reproducibility, accuracy verification. The contents of aluminum in two batches of mite allergen injection were detected by ICP-MS. The five samples of mite allergen injection were detected by ICP-MS and the colorimetric method Aluminum content. Results The linear range of ICP-MS was 0-100 ng / ml, r = 0.999 9, and the lowest detection limit was 0.111 ng / ml. The method was used to detect the relative standard of 6 times of 10 ng / ml standard solution The relative standard deviation (RSD) was 2.56%. The RSD value of the aluminum content in the six samples was 1.13%. The average recoveries of the aluminum content in the nine samples were 95.7% and the RSD was 1.37%. The method was used to detect the contents of aluminum in two samples of mite allergen injection and the results were in line with the standard requirements. The results of ICP-MS and colorimetric method for the determination of aluminum in five samples of mite allergen injection Consistent. Conclusion The ICP-MS method was developed for the determination of aluminum in mite allergen injection. The method is simple, rapid, accurate, reproducible and accurate, and has laid the foundation for the improvement of the quality standard of mite allergen injection basis.