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Improving the reliability of the iron concentration quantification for iron oxide nanoparticle suspensions: a two-institutions study
Analytical and Bioanalytical Chemistry ( IF 4.3 ) Pub Date : 2018-11-12 , DOI: 10.1007/s00216-018-1463-2
Rocio Costo , David Heinke , Cordula Grüttner , Fritz Westphal , M. Puerto Morales , S. Veintemillas-Verdaguer , Nicole Gehrke

Most iron oxide nanoparticles applications, and in special biomedical applications, require the accurate determination of iron content as the determination of particle properties from measurements in dispersions is strongly dependent on it. Inductively coupled plasma (ICP) and spectrophotometry are two typical worldwide used analytical methods for iron concentration determination. In both techniques, precise determination of iron is not straightforward and nanoparticle digestion and dilution procedures are needed prior to analysis. The sample preparation protocol has been shown to be as important as the analytical method when accuracy is aimed as many puzzling reported results in magnetic, colloidal, and structural properties are simply attributable to inadequate dissolution procedures. Therefore, a standard sample preparation protocol is needed to ensure the adequate and complete iron oxide nanoparticle dissolution and to harmonize this procedure. In this work, an interlaboratory evaluation of an optimized iron oxide nanoparticle digestion/dilution protocol was carried out. The presented protocol is simple, inexpensive, and does not involve any special device (as microwave, ultrasound, or other high-priced digestion devices). Then, iron concentration was measured by ICP-OES (performed in ICMM/CSIC-Spain) and spectrophotometry (NanoPET-Germany) and the obtained concentration values were analyzed to determine the most probable error causes. Uncertainty values as low as 1.5% were achieved after the optimized method was applied. Moreover, this article provides a list of recommendations to significantly reduce uncertainty in both sample preparation and analysis procedures.

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中文翻译:

改善氧化铁纳米颗粒悬浮液中铁浓度定量的可靠性:两个机构的研究

大多数氧化铁纳米颗粒应用以及特殊的生物医学应用都需要准确测定铁含量,因为根据分散体测量结果来确定颗粒性质非常依赖于此。电感耦合等离子体(ICP)和分光光度法是测定铁浓度的两种世界范围内常用的分析方法。在这两种技术中,铁的精确测定都不是一件容易的事,在分析之前需要进行纳米颗粒的消化和稀释程序。当精确度的目标是准确度时,样品制备规程与分析方法一样重要,因为许多令人困惑的磁性,胶体和结构性质的报告结果仅归因于不充分的溶解程序。所以,需要标准的样品前处理方案以确保氧化铁纳米颗粒充分充分溶解并协调该程序。在这项工作中,对优化的氧化铁纳米颗粒消化/稀释方案进行了实验室间评估。提出的协议简单,便宜,并且不涉及任何特殊设备(如微波,超声或其他高价消化设备)。然后,通过ICP-OES(在ICMM / CSIC-Spain中执行)和分光光度法(NanoPET-德国)测量铁浓度,并对获得的浓度值进行分析,以确定最可能的误差原因。应用优化方法后,不确定度值可低至1.5%。而且,

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更新日期:2018-11-12
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