微波消解-ICP-MS法同时测定软胶囊中10种痕量元素

为应对国家食品、药品安全的限量要求，采用微波消解法对软胶囊进行前处理，电感耦合等离子体质谱法（ICP-MS）同时测定软胶囊中铅、镉、砷、汞、铬、硒、铜、铁、锰和镍等10种痕量元素，并对测定条件进行了优化。结果表明：汞元素在0~10 μg/L范围内，其他元素在0~50 μg/L范围内的线性关系良好，线性相关系数r在0.999 4~0.999 9之间，方法检出限为0.011~0.21 μg/kg；考察了方法精密度，测定结果的相对标准偏差（RSD）为1.2%~5.7%；对各元素进行了3个不同浓度水平下的加标回收率实验，平均回收率为90.0%~110.0%。采用该方法测定了角鲨鱼肝NRCDOLT-3和奶粉GBW10017中的相应元素，测定结果与标准值无显著差异，验证了该方法测定多种不同基体软胶囊中痕量元素的实用性。

Simultaneous Determination of Ten Trace Elements in Soft Capsules by Microwave Digestion-ICP-MS

The contents of ten trace elements of lead, cadmium, arsenic, mercury, chromium, selenium, copper, iron, manganese and nickel in soft capsules were determined by inductively coupled plasma mass spectrometry (ICP-MS) with microwave digestion to fit the safety limits of China, and the analytical conditions were optimized. The results show that the linear ranges are 0.10 μg/L for mercury and 0.50 μg/L for the other elements with well the linear relationship, and the correlative coefficients are 0.999 4-0.999 9. The detection limits of the method are 0.011-0.21 μg/kg. The relative standard derivations (RSDs) are in the range of 1.2%-5.7%. The average recoveries at three levels are between 90.0% and 110.0%. The standard material NRCDOLT-3 Horn shark liver and GBW10017 milk powder are analyzed by the method, and the measured element values are in accord with the standard values. The method is suitable for the determination of trace elements in different matrix soft capsules.