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牛血清多元素分析的简单样品前处理方法的验证。

Validation of a simple sample preparation method for multielement analysis of bovine serum.

机构信息

Department of Animal Pathology, Veterinary Faculty, Universidade de Santiago de Compostela, Lugo Spain.

Faculty of Veterinary Medicine, Universidad Central del Ecuador, Quito, Ecuador.

出版信息

PLoS One. 2019 Feb 5;14(2):e0211859. doi: 10.1371/journal.pone.0211859. eCollection 2019.

Abstract

Here we propose a single acid digestion (SAD) sample preparation method for ICP-MS analysis of animal serum samples to determine trace element contents. The method was evaluated in comparison with a commonly used procedure involving dilution of samples in an alkaline solution (AKD). In the SAD procedure, aliquots (1 mL) of bovine serum samples were treated at low temperature with a mixture of concentrated nitric acid and hydrogen peroxide. Trace elements (As, B, Ba, Cd, Co, Cr, Cu, Fe, Hg, Li, Mn, Mo, Ni, Pb, Sb, Se, Sr, U, and Zn) were directly determined by ICP-MS analysis of diluted solutions of samples. Both methods were sufficiently sensitive to enable quantification of most trace elements, with the exception of the AKD method for Cd, Hg and Pb. The quality of the data was verified by using certified reference material. Good results were obtained for the SAD procedure and all elements, but recoveries were unacceptable with the AKD procedure for Se (recovery: 57%), Cd (154%) and Fe (139%). Strong associations (R2>0.90, P = 0.000) between the data obtained by both methods were demonstrated for the elements considered. The proposed SAD sample preparation method produced satisfactory results for determining most toxic and essential trace elements targeted in monitoring studies.

摘要

我们提出了一种用于 ICP-MS 分析动物血清样品中微量元素含量的单一酸消化(SAD)样品制备方法,与常用的稀释碱性溶液(AKD)的方法进行了比较。在 SAD 程序中,将牛血清样品的等分试样(1 mL)在低温下用浓硝酸和过氧化氢的混合物处理。通过对样品稀释溶液的 ICP-MS 分析,直接测定痕量元素(As、B、Ba、Cd、Co、Cr、Cu、Fe、Hg、Li、Mn、Mo、Ni、Pb、Sb、Se、Sr、U 和 Zn)。这两种方法都足够灵敏,能够定量大多数痕量元素,除了 AKD 方法无法定量 Cd、Hg 和 Pb。使用认证参考物质验证了数据的质量。SAD 程序和所有元素的结果都很好,但 AKD 程序的硒(回收率:57%)、镉(154%)和铁(139%)的回收率不可接受。两种方法得到的数据之间存在很强的相关性(R2>0.90,P=0.000),这对于监测研究中目标的大多数有毒和必需的痕量元素是如此。

我们提出的单一酸消化(SAD)样品制备方法可用于 ICP-MS 分析动物血清样品中的微量元素,结果令人满意。

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