摘要
目的:建立原子荧光光谱法测定活血止痛胶囊中砷、铅、汞含量的方法。方法:采用微波消解法对样品进行微波消解,使用氢化物发生-原子荧光光谱法测定6批活血止痛胶囊中砷、铅、汞含量。结果:砷、铅、汞分别在0~20、0~10、0~2μg·L^(-1)范围内呈良好的线性关系,相关系数r均≥0.9998;砷、铅、汞的检测限(LOD)分别为0.0569μg·L^(-1)、0.0476μg·L^(-1)、0.0052μg·L^(-1);加标回收率均在82.0%~108.9%;砷、铅、汞测定的精密度RSD分别为1.6%、1.4%、2.0%;8 h内稳定性RSD分别为3.9%、3.7%、4.9%;重复性RSD分别为2.5%、1.6%、3.7%。结论:原子荧光光谱法可以准确测定活血止痛胶囊中砷、铅、汞含量。该方法简便稳定,结果可靠,方法学验证结果良好,可以作为活血止痛胶囊中重金属检测的新方法,也为其他中成药中砷、铅、汞元素的限量控制提供一种新的思路。
Objective:To establish an atomic fluorescence spectrometry method for determining the content of arsenic,lead and mercury in Huoxue Zhitong capsules.Methods:The samples were digested by microwave digestion method.The content of arsenic,lead and mercury in 6 batches of Huoxue Zhitong capsules were determined by hydride generation-atomic fluorescence spectrometry.Results:Arsenic,lead and mercury showed good linear relationships within the ranges of 0-20,0-10 and 0-2μg·L^(-1) respectively,and the correlation coefficients(r)were all≥0.9998.The limit of detection(LOD)for arsenic,lead,and mercury were 0.0569μg·L^(-1),0.0476μg·L^(-1) and 0.0052μg·L^(-1) respectively.The spike recoveries were all between 82.0%and 108.9%.The RSDs of the determination precision of arsenic,lead and mercury were 1.6%,1.4%and 2.0%respectively.The RSDs of the stability within 8 hours were 3.9%,3.7%and 4.9%respectively.The RSDs of repeatability were 2.5%,1.6%and 3.7%respectively.Conclusion:Atomic fluorescence spectrometry can accurately determine the contents of arsenic,lead and mercury in Huoxue Zhitong capsules.This method is simple,stable and reliable,and has good methodological validation results.It can be used as a new method for the determination of heavy metals in Huoxue Zhitong capsules,and also provides a new idea for the limit control of arsenic,lead and mercury elements in other Chinese patent medicines.
作者
方静
钱晓翠
杨云松
朱琼
FANG Jing;QIAN Xiaocui;YANG Yunsong;ZHU Qiong(Taizhou Institute for Drug Control,Jiangsu Taizhou 225300,China)
出处
《中国医药导刊》
2025年第12期1343-1348,共6页
Chinese Journal of Medicinal Guide
基金
国家药品监督管理局化学药品杂质谱研究重点实验室开放课题(NMPA-KLIPCD-2023-06)。
关键词
原子荧光光谱法
活血止痛胶囊
砷
铅
汞
Atomic fluorescence spectrometry
Huoxue Zhitong capsules
Arsenic
Lead
Mercury
