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

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HNO和HO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0.5~500ng·mL^(-1)内与峰面积呈良好的线性关系(r≥0.99),在0.1,1和10μg3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24.8mg·kg^(-1);锶元素的含量则可高达67.6mg·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。

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 HNOand HOas 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 10μg,the average recoveries of most elements ranged from85.1%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 were100%,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.