检测螨变应原注射液中铝含量的电感耦合等离子体质谱法的建立及验证  

Development and verification of inductively coupled plasma-mass spectrometry for determination of aluminum content in mite allergen injection

作　　者：张瑾[1] 杨英超[1] 张影[1] 薄淑英[1] 王国柱[1] 辛晓芳[1] 王瑾[1] 

机构地区：[1]中国食品药品检定研究院,北京100050

出　　处：《中国生物制品学杂志》2014年第9期1207-1210,共4页Chinese Journal of Biologicals

基　　金：国家高技术研究发展计划(863计划;2012AA02A402)

摘　　要：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=0.9999;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 develop,verify and preliminarily apply an inductively coupled plasma-mass spectrometry（ICPMS）method for determination of aluminum content in mite allergen injection.Methods The samples were digested by closed-vessel microwave system,and determined for aluminum content by ICP-MS.ICP-MS was determined for linear range and minimum detection limit,and verified for precision,reproducibility and accuracy.The aluminum contents in two batches of mite allergen injection were determined by the developed ICP-MS.The aluminum contents in five batches of mite allergen injection were determined by the developed ICP-MS and colorimetry in the requirement for import of the product separately.Results The linear range of developed ICP-MS was 0 - 100 ng / ml,with a r value of 0.999 9,while the minimum detection limit was 0.111 ng / ml.The aluminum content in 10 ng / ml standard solution was determined by the method for 6 times,and the relative standard deviation（RSD） of determination results was 2.56%.The RSD of determination result of six samples was 1.13%.The total mean spike recovery rate of aluminum contents in nine samples was 95.7%,with a RSD of 1.37%.The aluminum contents in two batches of mite allergen injection determined by the developed method met the requirements for the product.The determination results of five batches of mite allergen injection were basically in agreement.Conclusion The ICP-MS for determination of aluminum content in mite allergen injection was developed,which was simple,rapid,precise,reproducible and accurate,and laid a foundation of improvement of quality standard for the injection.

关 键 词：螨变应原注射液 铝 电感耦合等离子体质谱 

分 类 号：O657.63[理学—分析化学]