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基于离散采样的流动注射进样作为 ICP-MS 中的一种引入系统,用于直接分析小体积的人血清样品。

Discrete sampling based-flow injection as an introduction system in ICP-MS for the direct analysis of low volume human serum samples.

机构信息

Trace Element, Spectroscopy and Speciation Group (GETEE), Strategic Grouping in Materials (AEMAT), Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, Universidade de Santiago de Compostela, Avenida das Ciencias, s/n, 15782 Santiago de Compostela, Spain.

Trace Element, Spectroscopy and Speciation Group (GETEE), Strategic Grouping in Materials (AEMAT), Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, Universidade de Santiago de Compostela, Avenida das Ciencias, s/n, 15782 Santiago de Compostela, Spain.

出版信息

Talanta. 2019 Jul 1;199:220-227. doi: 10.1016/j.talanta.2019.02.050. Epub 2019 Feb 11.

DOI:10.1016/j.talanta.2019.02.050
PMID:30952250
Abstract

Discrete sampling based on the flow injection options offered by advanced autosamplers has been tested and applied for the direct analysis of low volume samples (human serum) for multi-elemental purposes (simultaneous Al, Be, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Ni, Pb, Rb, Se, V, and Zn assessment). Serum samples (200 µL aliquots) were directly diluted to 2.0 mL with 1% (v/v) HNO, and discrete sampling operating conditions were optimized to allow cleaning, loading (300 µL injection loop), and measuring steps by using a volume lower than 2.0 mL (diluted serum sample). Matrix effect has been overcome by using the standard addition technique, and accurate results implied the use of kinetic energy discrimination (KED) mode (He as a collision gas) for measurements. The proposed method has been found to be reliable for serum samples analysis because of the low sample volume requirements, the minimal sample preparation required, and high sampling rate (each replicate analysis takes 2.50 min). In addition, validation results show good precision and accuracy (both analytical recovery and analysis of certified reference materials), and acceptable sensitivity. Applicability of the proposed method has been finally demonstrated by analysing several serum samples from healthy adults.

摘要

基于高级自动进样器提供的流动注射选项进行的离散采样已被测试和应用于直接分析低体积样品(人血清)进行多元素分析(同时评估 Al、Be、Ca、Cd、Co、Cr、Cu、Fe、K、Li、Mg、Mn、Mo、Ni、Pb、Rb、Se、V 和 Zn)。血清样品(200 µL 等分试样)直接用 1%(v/v)HNO3 稀释至 2.0 mL,通过使用低于 2.0 mL(稀释血清样品)的体积来优化离散采样操作条件,以允许进行清洗、加载(300 µL 进样环)和测量步骤。通过使用标准添加技术克服了基质效应,并且准确的结果意味着使用动能甄别(KED)模式(He 作为碰撞气体)进行测量。由于需要的样品体积低、所需的样品制备最少以及高采样率(每个重复分析需要 2.50 分钟),该方法已被发现可用于血清样品分析,是可靠的。此外,验证结果表明该方法具有良好的精密度和准确度(分析回收率和分析认证参考物质),并且具有可接受的灵敏度。该方法的适用性最后通过分析来自健康成年人的几个血清样本得到了证明。

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