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 0.481~116 μg·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 0.481-116 µg·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.
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