ICP-MS检测紫花地丁中37种无机元素含量

Content Determination of 37 Inorganic Element in Viola Yedoensis Makino by ICP-MS

关键词:  紫花地丁  ICP-MS  无机元素

Key words:  Viola yedoensis Makino  ICP-MS  inorganic element

摘要:

目的 测定紫花地丁中37种无机元素的含量，并建立多元素的电感耦合等离子体质谱（inductively coupled plasma mass spectrometry，ICP-MS）测定方法，初步探索研究紫花地丁药材中重金属元素的污染情况。方法 以HNO₃和H₂O₂作为消解溶剂，采用微波消解法前处理样品，通过ICP-MS同时测定紫花地丁中37种无机元素的含量。结果 37种无机元素在0.5~500 ng·mL^-1内与峰面积呈良好的线性关系（r ≥ 0.99），在0.1，1和10 μg 3个添加水平下，大多数元素的平均回收率介于85.1%~120.6%，RSD（n=6）<6%，仪器精密度和重复性的RSD值均<3%；19批紫花地丁中5种中国药典2015年版明确需要控制的有害重金属元素（铜、铅、砷、汞、镉）的检出率分别为铜和铅100%，砷和汞89.5%和10.5%，镉在所有样品中均未检出；钼元素和锶元素在19批样品检出率均为100%，且含量远远高于其他元素，钼元素的最高含量为24.8 mg·kg^-1；锶元素的含量则可高达67.6 mg·kg^-1。结论 该方法具有简便、快速、准确的优点，可用于紫花地丁中37种无机元素的含量测定。

Abstract:

OBJECTIVE To determine the content of 37 kinds of inorganic element in Viola yedoensis Makino, and to establish the multi-element inductively coupled plasma mass spectrometry(ICP-MS) method to preliminary explore the pollution of heavy inorganic element in Viola yedoensis Makino. METHODS With HNO₃ and H₂O₂ as digestion solvent, the samples were pretreated by microwave digestion method, and the contents of 37 kinds of inorganic element were determined simultaneously by ICP-MS method. RESULTS In the range of 0.5-500 ng·mL^-1, 37 inorganic element showed good linear relationship(r ≥ 0.99). At three supplemental levels of 0.1, 1 and 10 μg, the average recoveries of most elements ranged from 85.1% to 120.6%, the RSDs(n=6) were <6%, and the RSDs of instrument precision and reproducibility were <3%; the detection rates of 5 kinds of harmful heavy inorganic element(Cu, Pb, As, Hg, Cd) that needed to be controlled in the Chinese Pharmacopoeia(2015 Edition) of 19 batches of Viola yedoensis Makino were as followed:the detection rates of Cu and Pb were 100%, As and Hg were 89.5% and 10.5%, respectively, and Cd was not detected in all the samples. The detection rates of molybdenum and strontium in 19 batches of samples were 100%, and there content were much higher than other elements. The highest content of molybdenum was 24.8 mg·kg^-1. The content of strontium could be as high as 67.6 mg·kg^-1. CONCLUSION The method has the advantages of simplicity, rapidness and accuracy. It can be used for the determination of 37 kinds of inorganic element in Viola yedoensis Makino.