ICP-MS等三种测定蛹虫草硒含量方法的比较

Comparison of ICP-MS and Two Other Analytical Methods for Determination of Selenium Content in Cordyceps Militaris

采用微波消解法对试验样本进行消解,分别通过ICP-MS法、HPLC/荧光法和3,3-二氨基联苯胺比色法三种方法测定了富硒蛹虫草菌丝体中硒的含量,对上述几种硒含量测定方法的工作条件、检出限和精确度进行了对比研究。实验结果表明:ICP-MS法、HPLC/荧光法和3,3-二氨基联苯胺比色法的检出限分别为0.260 7,0.182 1和10.485 9μg.L-1,ICP-MS法的检出限最低,3,3-二氨基联苯胺比色法的检出限最高。在精密度方面,对同一样品以ICP-MS法测硒的标准差为最低,以3,3-二氨基联苯胺比色法测硒为最高。建议当分析样品中硒含量很低时,可选用HPLC/荧光法和ICP-MS法,如分析样品含硒量相对较大,可采用3,3-二氨基联苯胺比色法。

Samples were digested by microwave digestion. The selenium content in selenium enriched Cordyceps militaris was determined by ICP-MS method, HPLC/fluorometric method, and 3,3-diaminobenzidine method separately. And the detection conditions, the lowest detection limit and the relative standard deviation （RSD） of the three determination methods were compared. The detection conditions of the three methods for the detection of selenium content in selenium enriched Cordyceps rnilitaris were established. It was showed that the lowest detection limit of ICP-MS method, HPLC/fluorometric method, and 3,3- diaminobenzidine method was 0. 260 7, 0. 182 1 and 10. 485 9 μg ·L^-1 respectively, and this means that the lowest detection limit of ICP-MS method was the lowest and that of 3,3-diaminobenzidine method was the highest. For the same sample the rela- tive standard deviation （RSD） of ICP-MS method was the lowest and the RSD of 3,3-diaminobenzidine method was the highest. It was recommended that selenium content is determined by ICP-MS and HPLC/fluorometric method when the selenium in the sample is very low and by 3,3-diaminobenzidine method when the content is rather high.