微波消解-电感耦合等离子体质谱法测定植物样品中微量元素
Determination of Micro-amount of Elements in Plant Samples by Inductively Coupled Plasma-Mass Spectrometry with Microwave Digestion
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摘要: 采用过氧化氢-硝酸作溶剂,微波消解样品,外标方法校准,电感耦合等离子体质谱法同时测定植物样品中硼、镉、铜、钴、铬、钼、锂、镍、铅、镧、锗11个微量元素。确定了微波消解仪和等离子体质谱仪的最佳工作参数,研究了有机残留物和共存离子的干扰和消除方法,选择了各元素的测定同位素,以45Sc和103Rh双内标补偿基体效应,建立了样品测定方法。方法检出限(10 s)在5~150 ng/g,相对标准偏差(RSD,n=12)在1.27%~5.27%。对多种国家一级生物标准物质进行分析验证,测定值与标准值相符。方法适用于植物的果实、根、茎、叶等不同类型样品中多种微量元素的测定。
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关键词:
- 电感耦合等离子体质谱法; /
- 微波消解; /
- 微量元素; /
- 植物样品
Abstract: The plant samples were decomposed by microwave digestion using H2O2-HNO3as solvent. The external standard method was used for calibration. 11 micro-amount of elements of B, Cd, Cu, Co, Cr, Mo, Li, Ni, Pb, La and Ge in the plant samples were determined simultaneously by inductively coupled plasmamass spectrometry (ICP-MS). The parameters for microwave digestion and ICP-MS instrumental operation were optimized by experiments. The interference from organic residues and coexistent ions on determination of Pb, Cd, Ni and the interference eliminating methods were studied. 114Cd, 10B, 65Cu, 59Co, 52Cr, 98Mo, 7Li, 60Ni, 208Pb, 139La and 74Ge were chosen as determining isotopes and 103Rh and 45Sc were chosen as internal standards. The detection limits (10SD) of method for 11 elements were in a range of 5 ng/g to 150 ng/g. The method has been validated by determination of these elements in National Standard Reference materials and the results are in agreement with certified values with precision of 1.27% to 5.27%RSD (n=12). The method is suitable for determining these microamount of elements in fruits, roots, stems and leaves of different plants.-
Key words:
- inductively /
- coupled /
- plasma-mass /
- spectrometry
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