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Isotope Dilution Analysis of Se in Human Blood Serum by Using High-Power Nitrogen Microwave-Induced Plasma Mass Spectrometry Coupled with a Hydride Generation Technique

机译:高功率氮气诱导等离子体质谱-氢化物发生技术对人血清中硒的同位素稀释分析

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摘要

To establish a method for sensitive, accurate, and precise 'determination of Se in real samples, isotope dilution analysis using high-power nitrogen microwave-induced plasma mass spectrometry (N2 MW-IDMS) was conducted. In this study, freeze-dried human blood serum (Standard Reference Material, NIES No. 4) provided by NIES (National Institute for Environmental Studies) was used as a real sample. The measured isotopes of Se were ↑(78)Se and ↑(80)Se which are the major isotopes of Se. The appropriate amount of a Se spike solution was theoretically calculated by using an error multiplication factor (F) and was confirmed experimentally for the isotope dilution analysis. The mass discrimination effect was corrected for by using a standard Se solution for the measurement of Se isotope ratios in the spiked sample. However, the sensitivity for the detection of Se was not so good and the precision of the determination was not improved (2-3%) by N↓(2) MIP-IDMS with use of the conventional nebulizer. Therefore, a hydride generation system was connected to N↓(2) MIP-IDMS as a sample introduction system (HG-N↓(2) MIP-IDMS) in order to establish a more sensitive detection and a more precise determination of Se. A detection limit (3o) of 10 pg mL↑(-1) could be achieved, and the RSD was less than 1% at the concentration level of 5.0-10.0 ng mL↑(-1) by HG-N↓(2) MIP-IDMS. The analytical results were found to be in a good agreement with those obtained by the standard addition method using conventional Ar ICPMS.
机译:为了建立灵敏,准确和精确的测定实际样品中硒的方法,进行了使用高功率氮气微波诱导等离子体质谱(N2 MW-IDMS)的同位素稀释分析。在本研究中,使用NIES(国家环境研究所)提供的冻干人血清(标准参考材料,NIES No. 4)作为真实样品。硒的主要同位素为↑(78)Se和↑(80)Se。理论上,通过使用误差倍增因子(F)计算出适量的硒加标溶液,并通过实验确定用于同位素稀释分析。通过使用标准的硒溶液测量加标样品中硒的同位素比,可以校正质量歧视效应。但是,使用常规雾化器的N↓(2)MIP-IDMS不能很好地检测出Se的灵敏度,并且不能提高测定精度(2-3%)。因此,将氢化物生成系统连接到作为样品引入系统的N↓(2)MIP-IDMS(HG-N↓(2)MIP-IDMS),以便建立更灵敏的检测和更精确的Se测定方法。 HG-N↓(2)可以达到10 pg mL↑(-1)的检出限(3o),并且在5.0-10.0 ng mL↑(-1)浓度水平下RSD小于1%。 MIP-IDMS。发现分析结果与使用常规Ar ICPMS的标准添加方法获得的结果吻合良好。

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