摘要
目的探究电感耦合等离子体质谱(ICP-MS)法测定汞元素时加金与不加金对记忆效应和稳定性的影响,以及考察加金量。方法采用ICP-MS测定溶液中汞元素的量。射频功率为1 550 W,载气(高纯氩气)流速为1.05 L·min^(-1),等离子气体流速为15.0 L·min^(-1),蠕动泵转速0.2 r·s^(-1),采样深度8 mm,积分时间为0.1 s。结果汞溶液质量浓度在0.4 ng·m L^(-1)时开始形成较明显的记忆效应;汞溶液在不加任何稳定剂的情况下常温放置超过2 h后逐渐不稳定,相对标准偏差(RSD)逐渐变大,而加入金元素后在48 h内较为稳定,RSD在5%以内;金汞比为2∶1时就能够降低记忆效应,同时很好的保证其稳定性;汞元素标准溶液单独制备与其他元素混合制备并无区别。结论本实验对汞元素检测分析具有参考作用,为相关检测标准方法的修订和提高提供了技术支持。
OBJECTIVE To investigate the effect of adding gold when determing the memory effect and stability of mercury by ICP-MS,and determine the appropriate amount of gold.METHODS ICP-MS method was used to determine the amount of mercury in the solution.The RF power was 1 550 W,flow rate of carrier gas was 1.05 L·min^-1,plasma gas flow rate was 15.0 L·min^-1,peristaltic pump speed was 0.2 r·s^-1,and sampling depth was 8 mm.The integration time was 0.1 s.RESULTS Mercury solution began to demonstrate obvious memory effect at the concentration of 0.4 ng·m L^-1.It gradually became unstable and the coefficient of variation gradually increased after being placed at room temperature for more than 2 h in the absence of stabilizer.After adding gold,the mercury soulution was stable within 48 h,and the coefficient of variation was within 5%.When the ratio of gold to mercury was2∶1,the memory effect of mercury was decreaed,and its stability was well guaranteed.There was no difference when the mercury standard solution was prepared with or without other elements.CONCLUSION This study plays a reference role in the detection and analysis of mercury and provides technical support for the revision and improvement of relevant detection methods.
作者
李耀磊
金红宇
韩笑
马双成
LI Yao-lei;JIN Hong-yu;HAN Xiao;MA Shuang-cheng(College of Pharmacy,Beihua University,Jilin 132013, China;National Institutes for Food and Drug Control,Beijing 100050,China)
出处
《中国药学杂志》
CAS
CSCD
北大核心
2019年第1期53-57,共5页
Chinese Pharmaceutical Journal
基金
国家十二五"重大新药创制"课题"中药质量安全检测和风险控制技术平台"资助(2014ZX09304307-002)
作者简介
李耀磊,男,硕士,实习研究员研究方向:中药及天然药物外源性有害残留物质分析;通讯作者:韩笑,女,博士,副教授,研究方向:药物分析,Tel:(0432)64608281,E-mail:hanxiaorumeng@126.com.
