ICP-MS法测定冻干b型流感嗜血杆菌结合疫苗中多元素含量

Determination of multi elements in lyophilized Haemophilus influenzae b combined vaccine by ICP-MS

目的:建立一种电感耦合等离子体质谱法测定冻干b型流感嗜血杆菌结合疫苗中多元素的含量,对疫苗中含有的主要元素Ba、Ca、Cd、Si、Mg、B、Pb、As、Sb、Zn进行定量分析。方法:使用硝酸加高氯酸的混酸消解液,利用微波消解法进行样品前处理。对ICP-MS的参数进行调谐优化后,利用在线内标法消除疫苗样品的基体干扰。结果:该方法的相关系数均为0.999以上。利用该检测方法,回收率较好,在93.2%~101.9%之间。方法检测下限在0.481~116μg·L^(-1)之间,10种元素的精密度试验RSD在5%以内,除Si和B外,其他8种元素RSD在3%以内。对3个批次的实际疫苗样品进行了以上10种元素的测定,结果证明本方法有较好的可靠性。结论:本文提出的ICP-MS法快速、灵敏、准确,可以用于冻干b型流感嗜血杆菌结合疫苗样品10种元素的测定。

Objective:To establish an inductively coupled plasma mass spectrometry(ICP-MS)method for the determination of multi element content in lyophilized Haemophilus influenzae b combined vaccine,and to quantitatively analyze the main elements Ba、Ca、Cd、Si、Mg、B、Pb、As、Sb、Zn the vaccine.Methods:Using mixed acid solution of nitric acid and perchloric acid,sample pretreatment using microwave digestion.After tuning the ICP-MS parameters,The matrix interference of vaccine samples are eliminated by on-line internal standard method.Results:The correlation coefficient of this method was above 0.999.Using this method,better recovery was between 93.2%and 101.9%respectively.Methods:The detection limit was between 0.481-116μg·L^(-1),a precision test of 10 elements RSD was within 5%,The other 8 elements except Si and B were within 3%.Three batches of actual vaccine samples were tested for 10 elements,The results showed that this method had good reliability.Conclusion:This ICP-MS method is rapid,sensitive and accurate,that can be fully used for the determination of ten elements in lyophilized Haemophilus influenzae b combined vaccine samples.