桑白皮中21种无机元素的测定及其质量评价

Determination and Quality Evaluation of 21 Inorganic Elements in Mulberry Bark

为准确了解不同产区桑白皮中多种元素分布及含量情况,用65%硝酸溶液对其样品进行微波消解处理,后采用电感耦合等离子体质谱(ICP-MS/MS)法测定桑白皮样品中21种元素的含量。得到21种元素的线性关系良好,R^(2)>0.999,方法学考察实验的RSD均小于3%,加标回收率在91.3%~109%,RSD均小于4%;Al、Ga、Sr、Ba相比而言含量较高,且不同产区的特异性较明显;主成分分析中17批样品得到4个主成分,累计方差贡献率达87.380%,确定V、Co、Al、Li、As、Se、Pb、U、Zn、Cr、Cd、Ga、Ba、Cs、Ni等15种元素为桑白皮药材的特征元素;相关性分析可知,元素间的相关性较强,P≤0.05的元素与主成分分析的特征元素基本一致。参照2020年版《中国药典》中对中药材中有害元素的限量规定,发现桑白皮样品中Pb、Cd、As、Cu有害元素的含量均未超过限量要求。ICP-MS/MS能准确快速测定桑白皮中21种元素含量,这对评价不同产区桑白皮质量,完善桑白皮质量标准具有一定参考价值。

In order to accurately understand the distribution and contents of various elements in Mulberry bark from different production areas,the samples were subjected to microwave digestion with 65%nitric acid solution,and then inductively coupled plasma mass spectrometry(ICP-MS/MS)was used to determine the contents of 21 elements in the samples of Mulberry bark.The linear relationship of the 21 elements was good with R 2>0.999,and the RSD s of the methodology tests were all less than 3%.The recoveries of the spiked samples ranged from 91.3% to 109% with the RSDs less than 4%.Al,Ga,Sr and Ba were more abundant in comparison and were more specific to different production areas.The principal component analysis of the 17 batches of samples yielded four principal components with a cumulative variance contribution of 87.380%,and 15 elements,including V,Co,Al,Li,As,Se,Pb,U,Zn,Cr,Cd,Ga,Ba,Cs and Ni,were determined to be the characterizing elements of Mulberry bark.Correlation analysis showed that the correlation between the elements was strong,and the elements with P-value greater than 0.05 were basically consistent with the characteristic elements analyzed by principal component analysis.Referring to the content limit of harmful elements in traditional Chinese medicine of Pharmacopoeia People′s Republic of China(2020),It was found that the contents of Pb,Cd,As and Cu in the samples of Mulberry bark did not exceed the limits.ICP-MS/MS can accurately and quickly determine the content of 21 elements in Mulberry bark,which has certain reference value for evaluating the quality of Mulberry bark in different production areas and improving the quality standards of Mulberry bark.