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| ICP-AES测定海洋生物体中13种元素的微波消解条件优化 |
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孙玲玲1, 宋金明1, 林 强1, 孙 萱1, 于 颖1
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中国科学院 海洋研究所 分析测试中心
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| 摘要: |
| 报道了微波密闭消解正交试验条件优化电感耦合等离子体发射光谱法 (ICP-AES) , 同时测定8种海洋生物体中硒、铁、锰、锌、钙、镁、锶、砷、镉、铬、铜、铅和镍等 13 种元素含量的实验结果。优化后的样品消解条件为加入的VHNO3:VH2O2 = 6.0 mL: 1.0 mL, 第二步程序升温温度为 170℃, 消解时间 20 min; 测定标准曲线相关系数大于 0.999, 相对标准偏差为 0.30%～2.55%, 加标回收率为92.0%～104.8%, 方法检出限为0.0010～0.0468 μg/g。结果表明, 优化后方法测定操作简便、具有高的灵敏度、准确度和精密度, 且能多元素同时测定, 适合于海洋生物样品中这些元素含量的准确测定, 并可为评估海产品食用安全提供科学依据。 |
| 关键词: 条件优化 微波消解 ICP-AES 测定 |
| DOI：10.11759/hykx20130818001 |
| 分类号: |
| 基金项目:国家自然科学基金资助资目(41306070) |
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| Optimization of microwave digestion conditions for 13 elements in marine organisms by ICP-AES |
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| Abstract: |
| Herein, thirteen elements including Se, Fe, Mn, Zn, Ca, Mg, Sr, As, Cd, Cr, Cu, Pb and Ni in eight kinds of marine organisms were determined by using microwave digestion technique, and applying Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES). The conditions of microwave digestion were optimized through orthogonal experiment design. The optimum conditions were as follows: the volume ratio of HNO3:H2O2︰6︰1, digestion temperature: 170 ℃, and digestion time: 20 min. The correlation coefficients of linear regression equation for all elements were above 0.999. The recovery rate of the method was in the range of 92.0%～104.8%, and the relative standard deviations were between 0.30% and 2.55%. The detection limit of the method ranged from 0.0010 μg/g to 0.0468 μg/g. The results indicated that the optimized method was convent, sensitivity, accurate and precision, and also can be used for simultaneous multi-element detection. It was suitable for determination of these elements in marine organisms, and also provided scientific foundation for evaluation of safety of seafood. |
| Key words: Condition optimization Microwave digestion ICP-AES Determination |
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