仿生提取-电感耦合等离子体-质谱法测定柏子养心片中可溶性重金属

Determination of Soluble Heavy Metals in Baizi Yangxin Tablets by Inductively Coupled Plasma Mass Spectrometry with Bionic Extraction and Microwave Digestion Technology

国家食品药品监督管理总局的2014年国家药品抽验计划将柏子养心片定为抽验品种,本实验利用人工胃液仿生提取样品可溶性重金属,通过微波消解技术对提取液进行消解处理,建立了仿生提取-ICP-MS法测定18批柏子养心片中Co,Cr,Cu,Ba,Cd,Mn,Ni,Pb,Hg,Sr,Zn 11种可溶性重金属的含量的分析方法。本方法各元素标准系列线性回归方程的相关系数为0.9989~1.0000,检出限为0.19~5.6μg/L,方法的重复性RSD值均小于6.2%,精密度的RSD值均小于5.6%,加标回收率在87.7%~101.9%之间,满足检测要求。参照《药用植物及制剂进出口绿色行业标准》规定的重金属限量标准,18批样品中Pb,Cd,Cu均未超过标准,Hg含量平均值为7.68 mg/kg,超过标准值。仿生提取-ICP-MS法的建立为柏子养心片的安全性研究提供参考依据。

Baizi Yangxin tablets are common Chinese medicine used for the treatment of heart palpitations, insomnia and irritable forgetful. To evaluate the total amount of heavy metals evaluation, artificial gastric juice was used as juice samples and the extracted soluble heavy metals were extracted by microwave digestion technology. An analytical method of bionic extraction microwave digestion with inductively coupled plasma mass spectrometry （ ICP-MS ） was established for the determination of trace metals, such as Co, Cr, Cu, Ba, Cd, Mn, Ni, Pb, Hg, Sr and Zn, in 18 batches of Baizi Yangxin tablets. The correlation coefficient of linear regression equation for different elements ranged from 0. 9989 to 1. 0000, the detection limit was 0. 19-5. 6 μg / L, and the repeatability of the method was less than 6. 2% , the precision of the RSD value was less than 5. 6% , and the recovery rate was 87. 7% -101. 9% . According to “the standard of the heavy metal in the standard of import and export of medicinal plants and preparations”, the contents of Cd, Cu and Pb in the 18 batches were not exceed the standard, but the Hg content （7. 68 mg / kg） exceeded the standard value. The bionic extraction-ICP-MS method provide a reference basis for the safety of the proprietary Chinese medicine＆#39;s study.