电感耦合等离子体质谱法测定新型冠状病毒灭活疫苗(Vero细胞)的铝含量

Determination of aluminum in COVID-19 inactivated vaccine(Vero Cell)by inductively coupled plasma mass spectrometry

目的:建立测定新型冠状病毒灭活疫苗(Vero细胞)铝含量的电感耦合等离子体质谱(ICP-MS)法。方法:以钪为内标元素,用2%硝酸溶液稀释样品,采用ICP-MS法进行测定,选择碰撞池模式(KED),射频功率1.6 kW,等离子体流量14.99 L·min^(-1),雾化气流速1.02 L·min^(-1),辅助气流量1.20 L·min^(-1),蠕动泵转速:-35 r·min^(-1),氦气流速5 mL·min^(-1),积分时间2 s,跳峰模式,重复次数3次。并进行相关的方法学验证。结果:铝元素质量浓度在0~2 mg·L^(-1)范围内线性关系良好(r=0.9999);检测限为0.0739μg·L^(-1),定量限为0.2462μg·L^(-1);精密度RSD(n=8)为0.70%;重复性RSD(n=8)为3.0%;平均回收率(n=8)为106.7%,RSD为2.1%。结论:ICP-MS法操作简单、快速,准确度和重复性好,可用于新冠病毒灭活疫苗(Vero细胞)的铝含量测定。

Objective:To establish a method for the determination of aluminum element in COVID-19 inactivated vaccine(Vero Cell)by inductively coupled plasma mass spectrometry.Methods:Scandium was as the internal standard element and the sample was diluted with 2%nitric acid solution.ICP-MS method was used for determination.The collision cell mode(KED)was selected,with a radiofrequency power of 1.6 kW,a plasma gas flow rate of 14.99 L·min^(-1),a nebulizer gas flow rate of 1.02 L·min^(-1),an auxiliary gas flow rate of 1.20 L·min^(-1),a peristaltic pump speed of-35 r·min^(-1),a helium flow rate of 5 mL·min^(-1),an integration time of 2 s,and a peak-jumping mode with 3 repetitions.The relevant methodological validation was conducted.Results:There was a good linear relationship for aluminum element within the range of 0-2 mg·L^(-1)(r=0.9999),the limit of detection was 0.0739μg·L^(-1),the limit of quantifi-cation was 0.2462μg·L^(-1).RSD of precision tests(n=8)was 0.70%.And RSD of repeatability tests(n=8)was 3.0%.The average recovery(n=8)was 106.7%with an RSD of 2.1%.Conclusion:The established ICP-MS method is simple,rapid,accurate and reproducible,and can be used for the determination of aluminum content in the COVID-19 inactivated vaccine(Vero cell).