电感耦合等离子体-质谱法测定原淀粉中的14种杂质元素  

Determination of 14 elemental impurities in starch by ICP-MS

作　　者：胡淑君 叶秀金[1] 郭雅娟 陈英[1] HU Shujun;YE Xiujin;GUO Yajuan;CHEN Ying(CFDA Key Laboratory of Quality Control and Evaluation of Pharmaceutical Excipients,Guangdong Institute for Drug Control,Guangzhou,Guangdong,510663 P.R.China)

机构地区：[1]广东省药品检验所国家药品监督管理局药用辅料质量控制与评价重点实验室,广东广州510663

出　　处：《华西药学杂志》2022年第4期448-452,共5页West China Journal of Pharmaceutical Sciences

基　　金：国家药典委员会项目(ZG2018-5-04);广东省科技计划项目(2018B020207008)。

摘　　要：目的参照ICH Q3D指导原则,测定原淀粉类药用辅料中锂、钒、铬、钴、镍、铜、砷、硒、银、镉、钡、汞、铊、铅等14种杂质元素的残留量。方法采用电感耦合等离子体-质谱法,载气为He,等离子体模式为HMI-8,载气流量0.8 L·min^(-1),雾化气流量0.8 L·min^(-1),辅助气流量0.8 L·min^(-1),等离子气流量15.0 L·min^(-1),蠕动泵转速0.1 r·min^(-1),雾化室温度2.0℃,内标法测定含量。结果14种元素杂质的r均大于0.998;加样回收率为79.0%~115.2%,RSD为1.90%~8.40%;精密度的RSD为0.80%~6.70%;44批样品中14种元素杂质的含量均在限度范围内。结论所用方法灵敏度高,精密度、准确度良好,能够很好地控制原淀粉中的元素杂质,为原淀粉及药用辅料的风险评估提供参考,更好地保障药品安全。OBJECTIVE To determine 14 elemental impurities in starch pharmaceutical excipients in reference with ICH Q3D guidelines.METHODS ICP-MS method was used for elemental impurity testing in starch with carrier gas of He.The plasma mode was set as HMI-8.The power of radio frequency was 1600 W.The carrier gas flow rate was 0.8 L·min^(-1).The nebulizer gas flow was 0.8 L·min^(-1).The auxiliary gas flow was 0.8 L·min^(-1).The plasma gas flow was 15.0 L·min^(-1).The speed of nebulizer pump was 0.1 r·min^(-1).The temperature of atomizer chamber was 2.0℃with internal standard method.RESULTS Regression coefficients of the standard curve of the 14 elemental impurities were all over 0.998.The recovery rates were within the range of 79.0%^(-1)15.2%.The RSD of the recovery rate was between 1.90%-8.40%.The RSD of the precision rate was between 0.80%-6.70%.The contents of the 14 elemental impurities in 44 batches of samples all met the requirements.CONCLUSION This method is highly sensible,reproducible and accurate,which can well control the element impurities in starch.It provides reference for the risk assessment of starch pharmaceutical excipients and helps to ensure the drug security.

关 键 词：ICH Q3D 淀粉 药用辅料 元素杂质 电感耦合等离子体-质谱法 内标法 风险评估 药品安全 

分 类 号：R917[医药卫生—药物分析学]