ICP-MS法同时测定重组乙型肝炎疫苗中的12种元素杂质  

Simultaneous determination of 12 elemental impurities in recombinant hepatitis B vaccine by ICP-MS

作　　者：邵天舒 李文东 赵璇 郭雷 SHAO Tianshu;LI Wendong;ZHAO Xuan;GUO Lei(NMPA Key Laboratory for Safety Research and Evaluation of Innovative Drugs,Beijing Institute for Drug Control,Beijing,102206 P.R.China)

机构地区：[1]北京市药品检验研究院、国家药品监督管理局创新药物安全研究与评价重点实验室,北京102206

出　　处：《华西药学杂志》2023年第2期176-180,共5页West China Journal of Pharmaceutical Sciences

摘　　要：目的同时测定重组乙型肝炎疫苗中12种元素杂质的含量。方法采用电感耦合等离子体质谱内标法。载气(氩气)流量1.02 L·min^(-1),碰撞气(氦气)流量4.5 L·min^(-1),等离子体气流量18 L·min^(-1),射频功率1.35 kW,采样锥截取深度为65 mm,积分时间为1.5 s,数据采样为跳峰模式,样品重复测3次,取平均值。结果0.05~100μg·L^(-1)镉、铅、砷、钴、钒、镍、铊、银、铜、铬、钡、钨与响应值呈良好的线性关系(r>0.9994),定量限0.4590~40 ng·L^(-1),检测限0.1377~12 ng·L^(-1)。精密度试验RSD不超过2.50%,重复性试验RSD不超过8.90%,平均加样回收率78.5%~114.3%,RSD为0.10%~4.40%。结论所用方法快速、简便、准确,线性、精密度、重复性良好,可用于同时测定重组乙型肝炎疫苗中的元素杂质。OBJECTIVE To simultaneously determine the 12 elements in recombinant hepatitis B vaccine.METHODS ICP-MS with internal standard was adopted.The radiofrequency power was 1350 W;the flow rate of carrier gas(argon)and collision gas(helium)was 1.02 L·min^(-1) and 4.5 L·min^(-1) respectively.The integration time was 1.5 s.The plasma gas flow rate was 18 L·min^(-1).The sampling depth was 65 mm.The data sampling mode was peak-jump acquisition mode,and the data collection was repeated 3 times for the average value.RESULTS The linear ranges of Cd,Pb,As,Co,V,Ni,Tl,Ag,Cu,Cr,Ba,W were between 0.05μg·L^(-1) and 100μg·L^(-1)(r>0.9994).The limits of quantitation were 0.4590-40 ng·L^(-1),and the limits of detection were 0.1377-12 ng·L^(-1).The RSDs of precision test was less than 2.50%while the RSDs of repeatability test was below 8.90%.The spike recoveries ranged from 78.5%to 114.3%,with RSDs between 0.10%and 4.40%.CONCLUSION The method is rapid,simple and accurate.The linearity,precision and repeatability of this method are also good.It is suitable for the simultaneous content determination of elemental impurities in recombinant hepatitis B vaccine.

关 键 词：重组乙型肝炎疫苗 元素杂质 电感耦合等离子体质谱法 内标法 痕量 限量检查 安全性 浸出 

分 类 号：R917[医药卫生—药物分析学]