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Determination of bromine and iodine in shrimp and its parts by ICP-MS after decomposition using microwave-induced combustion

机译:微波诱导燃烧分解-ICP-MS法测定虾及其部位中的溴和碘

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A digestion method based on microwave-induced combustion (MIC) was developed for bromine and iodine determination in shrimp and its parts (shells and head, and tissue) by inductively coupled plasma mass spectrometry (ICP-MS). Ammonium nitrate solution was used as an igniter for combustion and vessels were pressurized with O2 at 20 bar. Solutions of (NH4)2CO3 (50 or 100 mmol La?’1) and NH4OH (25, 50, 75 or 100 mmol La?’1) were evaluated as absorbing media for Br and I. Better results were obtained for Br and I determination using 50 mmol La?’1 NH4OH as absorbing medium. Using this solution, blanks were always negligible and memory effects were virtually absent. The accuracy of the proposed MIC method was evaluated using a reference material (NIST 8414) with agreement better than 99% for both analytes. The limits of detection by MIC and further ICP-MS determination (Br: 0.12 ??g ga?’1; I: 0.001 ??g ga?’1) were better than those obtained when the extraction procedure was used. Additionally, a microwave-assisted alkaline extraction method was also evaluated using 0.11 mol La?’1 TMAH as extractant solution. However, alkaline extraction was only feasible for shrimp tissue and not for whole shrimp or shells. Decomposition using MIC allowed the determination of Br and I by ICP-MS in shrimp and the respective distribution of these elements in shells and head, and in tissue avoiding the use of concentrated digestion or extraction solutions.
机译:开发了一种基于微波诱导燃烧(MIC)的消解方法,通过电感耦合等离子体质谱法(ICP-MS)测定虾及其部位(壳,头部和组织)中的溴和碘。硝酸铵溶液用作燃烧的点火器,并用20 bar的氧气对容器加压。评价了(NH4)2CO3(50或100 mmol La?'1)和NH4OH(25、50、75或100 mmol La?'1)的溶液作为Br和I的吸收介质.Br和I获得了更好的结果用50mmol La 2 NH 4 OH作为吸收介质测定。使用此解决方案,空白始终可以忽略不计,并且几乎没有记忆效应。使用参考材料(NIST 8414)评估了拟议的MIC方法的准确性,两种分析物的一致性均优于99%。通过MIC和进一步ICP-MS测定的检出限(溴:0.12 g·g ga -1; I:0.001 g·g ga -1)优于使用萃取程序获得的限度。此外,还使用0.11 mol La?1 TMAH作为萃取液评估了微波辅助碱萃取法。但是,碱提取仅对虾组织可行,而对整只虾或壳没有可行性。使用MIC进行分解可通过ICP-MS测定虾中的Br和I,以及这些元素在壳和头中以及在组织中的各自分布,从而避免使用浓缩的消化或提取溶液。

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