四种前处理方法对电感耦合等离子体质谱测定植物样品中27种微量元素的影响
Comparison of Different Digestion Procedures for Elemental Determination in Plant Samples by Inductively Coupled Plasma-Mass Spectrometry
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摘要: 采用HNO3-HClO4-HF常压消解、HNO3-H2O2-HF高压密闭消解、HNO3-H2O2微波消解,干法灰化后残渣用HNO3-HF-HClO4溶解等四种方法对植物样品进行前处理,使用电感耦合等离子体质谱(ICP-MS)对植物样品中的27种元素进行定量分析,探讨了不同前处理方法对ICP-MS测定植物样品中微量元素的影响。分析结果表明: HNO3-HClO4-HF常压消解使用大量试剂,污染环境,造成空白值高;在常压体系中HClO4的加入能提高样品的消解效率,但赶酸不完全,会造成复合离子对钒和砷的干扰;干法灰化过程中某些元素(硼、汞等)会损失;常压消解和高压密闭消解中加入HF能有效地提高铍、稀土、钇、钛、锑、铀等元素的回收率,但在蒸干赶HF的过程中,会造成硼和汞的损失,并且钢套的生锈会造成铬、镍空白值高。尽管没有一种方法能适用于所有元素的分析,但相比较而言,HNO3-H2O2微波消解体系操作简单,大部分元素(除铍、钛、锑、铋、稀土)能得到满意的结果,精密度(RSD)均小于10%(n=10),相对误差(RE)为-4.6%~13.6%。
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关键词:
- 植物样品 /
- 微量元素 /
- 样品消解方法 /
- 电感耦合等离子体质谱法
Abstract: The overall aim of this study was to identify the influence of different digestion methods for the determination of trace elements by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) in various plant samples. Four digestion procedures including HNO3-HClO4-HF at normal pressure, HNO3-H2O2-HF in a pressurized vessel, microwave-assisted digestion with HNO3-H2O2, and HNO3-HClO4-HF after dry ashing were applied for the decomposition of plant samples. Quantitative analysis for the 27 elements in three Certified National Reference Materials GBW 07603, GBW 07604 and GBW 07605 was measured by using ICP-MS. It was demonstrated that the results of some volatile elements (Hg, B, etc.) were significantly lower than certified concentration values, which was consistent with these elements being volatile at high temperatures during ashing. Using a large amount of reagents in normal pressure digestion pollutes the environment, and results in a high blank value. The efficiency of digestion was promoted by using HClO4 in a normal pressure system. However, HClO4 could not be removed completely nor the interferences to the determination of V and As by the complex ion with Cl-. Using HF in digestion at normal pressure and in a pressurized vessel improved recoveries of the REEs, Be, Ti, Sb and U etc. However, the B and Hg volatilized during the procedure of removing HF with heating. A rusty steel vessel caused high blank values of Ni and Cr. Although none of the methods were good enough to provide accurate determinations for all elements in the Certified Reference Materials, a relatively simple method of HNO3 and H2O2, digested in a microwave oven yielded the most acceptable results with a precision of less than 10% RSD and relative error of -4.6%-13.6%, except for Be, Ti, Sb, Bi and REEs. -
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梁立娜,李中阳,陈登云,江桂斌. ICP-MS技术测定生物样品中重金属的前处理方法研究[J].环境化学,2003,22(1): 99-100. 陈杭亭,曹淑琴,曾宪津.电感耦合等离子体质谱方法在生物样品分析中的应用[J].分析化学,2001,29(5): 592-600. 李文龙,荆淼,陈军辉,陈登云,王小如.微波消解-ICP-MS测定40种中药材中的5种有毒元素[J].分析试验室,2008,27(2): 6-9. 李刚,高明远,诸堃.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[J].岩矿测试,2010,29(1): 17-22. Ashoka S, Peake B M, Bremner G, Hageman K J, Reid M R. Comparison of digestion methods for ICP-MS determination of trace elements in fish tissues [J]. Analytica Chimica Acta,2009,653: 91-99. Ashoka S, Peake B M, Bremner G, Hageman K J, Reid M R. Comparison of digestion methods for ICP-MS determination of trace elements in fish tissues [J]. Analytica Chimica Acta,2009,653: 91-99.
Millour S, Noёl L, Kadar A, Chekri R, Vastel C, Guérin T. Simultaneous analysis of 21 elements in foodstuffs by ICP-MS after closed-vessel microwave digestion: Method validation[J]. Journal of Food Composition and Analysis, 2011,24(1): 111-120. Millour S, Noёl L, Kadar A, Chekri R, Vastel C, Guérin T. Simultaneous analysis of 21 elements in foodstuffs by ICP-MS after closed-vessel microwave digestion: Method validation[J]. Journal of Food Composition and Analysis, 2011,24(1): 111-120.
López F J, Garcia M D, Morito N P, Vidal J L. Determination of heavy metals in crayfish by ICP-MS with a microwave-assisted digestion treatment[J]. Ecotoxicology and Environmental Safety, 2003,54(2): 223-228. López F J, Garcia M D, Morito N P, Vidal J L. Determination of heavy metals in crayfish by ICP-MS with a microwave-assisted digestion treatment[J]. Ecotoxicology and Environmental Safety, 2003,54(2): 223-228.
Mesko M F, Hartwig C A, Bizzi C A, Pereira J S F, Mello P A, Flores E M M. Sample preparation strategies for bioinorganic analysis by inductively coupled plasma mass spectrometry [J]. International Journal of Mass Spectrometry, 2011,307(1-3): 123-136. Mesko M F, Hartwig C A, Bizzi C A, Pereira J S F, Mello P A, Flores E M M. Sample preparation strategies for bioinorganic analysis by inductively coupled plasma mass spectrometry [J]. International Journal of Mass Spectrometry, 2011,307(1-3): 123-136.
Pick D, Leiterer M, Einax J W. Reduction of polyatomic interferences in biological material using dynamic reaction cell ICP-MS[J]. Microchemical Journal, 2010, 95(2): 315-319. Pick D, Leiterer M, Einax J W. Reduction of polyatomic interferences in biological material using dynamic reaction cell ICP-MS[J]. Microchemical Journal, 2010, 95(2): 315-319.
李冰,杨红霞.电感耦合等离子体质谱原理和应用[M].北京: 地质出版社,2005. 王小平.不同分解方法对ICP-AES测定植物样品中元素含量的影响[J].光谱学与光谱分析,2005,25(4): 563-566. Qi L, Hu J, Gregoire D C. Determination of the trace elemens in granites by inductively coupled plasma mass spectrometry[J]. Talanta, 2000,51: 507-513. Qi L, Hu J, Gregoire D C. Determination of the trace elemens in granites by inductively coupled plasma mass spectrometry[J]. Talanta, 2000,51: 507-513.
孙德忠,何红蓼,温宏利,马生凤,巩爱华,殷绍泉.干灰化结合偏硼酸锂碱熔灰分ICP-AES测定生物样品中的硅铝等元素[J].光谱学与光谱分析,2008,28(1): 195-199. 李冰,马新荣,杨红霞,何红蓼.封闭酸溶-电感耦合等离子体原子发射光谱法同时测定地质样品中硼砷硫[J].岩矿测试,2003,22(4): 241-247. 王小平,高伟健,项苏留.植物样品消解后残留颗粒物元素组成研究[J].光谱学与光谱分析,2006,26(2): 348-352.
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