半消解-电感耦合等离子体质谱法测定分心木中锰、铜、锶和钡

本研究建立了半消解-电感耦合等离子体质谱法测定分心木中锰、铜、锶和钡元素,分析了消解液种类、硝酸体积和消解时间对样品中微量元素回收率的影响。在优化的条件下,各待测元素的标准曲线呈良好的线性关系,相关系数大于0.9998,检出限为0.037~0.11μg/L,相对标准偏差为0.45%~2.99%,平均加标回收率为95.7%~109.3%。使用该方法检测国家标准物质GBW10020柑橘叶,结果均在标准参考值范围内。t检验表明,该方法与微波消解法的测定结果无显著性差异。该方法操作简单、快速、结果准确,可为分心木中微量元素的检测提供方法参考。

Determination of Mn,Cu, Sr and Ba in Diaphragma Juglandis Fructus by Semi-Digestion-ICP-MS

Diaphragma Juglandis Fructus, the dry wood diaphragm tissue that grows inside the Juglans regia L., has been used for treating many diseases such as kidney asthenia, chronic glomerulonephritis and chronic renal insufficiency. Analytical methods for determination of trace elements in Diaphragma Juglandis Fructus have been reported. The main pretreatment method is wet digestion, which has some shortcomings such as tedious preparation steps, long digestion time and high chemical reagent consumption. Therefore, it is essential to develop an appropriate analytical methodologies for determination of trace elements in Diaphragma Juglandis Fructus. In this work, a method of semi digestion inductively coupled plasma mass spectrometry (ICP MS) was developed for the determination of manganese, copper, strontium and barium trace elements in Diaphragma Juglandis Fructus. In order to get good digestion efficiencies of the target elements, the important factors affecting the semi digestion procedure were discussed, such as nature of acid solution, volume of concentrated nitric acid and digestion time. Finally, 0.2 g Diaphragma Juglandis Fructus sample treated with 2 mL of concentrated nitric acid and then transferred to graphite digestion instrument(120 ℃) for 10 min. Then the digestion solution was filtered by 045 μm polyethersulfone filtration membrane and detected by ICP MS. Results of semi digestion method were compared with those obtained with microwave assisted digestion as reference method. The results showed that the standard curve of each element has a good linear correlation with a coefficient higher than 0999 8. The detection limits are 0037 011 μg/L. The relative standard deviations (RSDs) and average recoveries are in the range of 045% 299% and 957% 1093%, respectively. The results of national standard substance (GBW 10020 citrus leaf) are all within the standard reference value range. The results of t test indicated that difference in the results from semi digestion and microwave assisted digestion is not significant. The method is simple, rapid and accurate, which is suitable for determination of the 4 trace elements in Diaphragma Juglandis Fructus.