Bromine, Chlorine, and Iodine Determination in Soybean and its Products by ICP-MS After Digestion Using Microwave-Induced Combustion
Bromine, Chlorine, and Iodine Determination in Soybean and its Products by ICP-MS After Digestion Using Microwave-Induced Combustion
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DOI：
10.1007/s12161-012-9511-6
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发表时间：
2013-08-01
影响因子：
2.9
通讯作者：
Moraes Flores, Erico Marlon
中科院分区：
文献类型：
--
作者：
Pereira Barbosa, Jose Tiago;Moreira Santos, Clarissa Marques;Moraes Flores, Erico Marlon
建立了微波诱导燃烧（MIC）消解-电感耦合等离子体质谱（ICP-MS）测定大豆及其制品中溴、氯和碘的方法。将样品压制成颗粒，并使用加压氧气（20巴）和硝酸铵溶液（50 μ L的6 mol L-1）作为点火剂燃烧。分析物被吸收在碱性溶液（100 mmol L-1 NH 4 OH），和5分钟的回流步骤，微波功率为1,400 W，燃烧后，以提高分析物的回收率。对于通过ICP-MS测定Cl，使用动态反应池，以氨作为反应气体。使用有证参比物质（CRM）和加标样品评价准确度。使用MIC，对于相似组成的经认证参比物质（美国国家标准与技术研究院（NIST），玉米麸皮和NIST，全脂牛奶）的所有分析物，与CRM值和加标回收率的一致性均高于95%。检测限分别为0.03，1.2，和0.002微克克（-1）溴，氯，和I，分别。经MIC程序处理后，得到的样品中残余碳含量低于0.5%。空白总是可以忽略不计，没有观察到记忆效应。MIC消化允许在25分钟内每次运行处理多达8个样品，消化效率高，为ICP-MS进一步测定溴、氯和碘提供了合适的介质。
A method for bromine, chlorine, and iodine determination in soybean and related products was developed by inductively coupled plasma mass spectrometry (ICP-MS) after digestion by microwave-induced combustion (MIC). Samples were pressed as pellets and combusted using pressurized oxygen (20 bar) and ammonium nitrate solution (50 mu L of 6 mol L-1) as the igniter. Analytes were absorbed in alkaline solution (100 mmol L-1 NH4OH), and a reflux step of 5 min, microwave power of 1,400 W, was applied after combustion in order to improve analyte recoveries. For Cl determination by ICP-MS, a dynamic reaction cell was used with ammonia as the reaction gas. The accuracy was evaluated using certified reference materials (CRMs) and spiked samples. Using MIC, the agreement with CRM values and spike recoveries was higher than 95 % for all analytes for certified reference materials of a similar composition (National Institute of Standards and Technology (NIST), corn bran and NIST, whole milk). Limits of detection were 0.03, 1.2, and 0.002 mu g g(-1) for Br, Cl, and I, respectively. The residual carbon content in the digests obtained after MIC procedure was lower than 0.5 %. Blanks were always negligible and no memory effects were observed. Digestion by MIC allowed processing up to eight samples by each run in 25 min with high efficiency of digestion providing a suitable medium for further bromine, chlorine, and iodine determination by ICP-MS.