Measurement uncertainty of selenium determination in the reference material Seronorm Trace Elements Serum by hydride generation atomic fluorescence spectrometry

 An analytical result is not considered to be complete without a statement of the measurement uncertainty associated with it. Evaluation of measurement uncertainty is therefore an essential part of every determination. In the present study the measurement uncertainty of the result of determination of selenium in the reference material Seronorm Trace Elements Serum was studied. The combination of a digestion procedure using sulfuric acid, V₂O₅ in H₂SO₄ and hydrogen peroxide and the continuous flow approach of hydride generation atomic fluorescence spectrometry (HG-AFS) detection was used for selenium determination. The total uncertainty budget was calculated with the help of the GUM Workbench program, in which computations follow the rules of the ’ISO guide to the expression of uncertainty in measurement’. The major sources of uncertainty were found to be due to the recovery of the procedure, measurement of peak heights and the purity of Na₂SeO₃. A selenium mass fraction of 77.1±4.8 ng/g (with a coverage factor of 2.1, 95% probability) was determined, which is comparable with the recommended value of 80 ng/g. Received: 13 September 2002 Accepted: 23 December 2002 Acknowledgements We would like to thank Tinkara Buˇcar, B.Sc. for useful discussions and the IAEA Vienna, for financial support of the project 11553/RO. Presented at CERMM-3, Central European Reference Materials and Measurements Conference: The function of reference materials in the measurement process, May 30–June 1, 2002, Rogaška Slatina, Slovenia Correspondence to V. Stibilj     

Folate binding protein—Outlook for drug delivery applications

Serum proteins represent an important class of drug and imaging agent delivery vectors. In this minireview, key advantages of using serum proteins are discussed, followed by the particular advantages and challenges associated with employing soluble folate binding protein. In particular, approaches employing drugs that target folate metabolism are reviewed. Additionally, the slow-onset, tightbinding interaction of folate with folate binding protein and the relationship to a natural oligomerization mechanism is discussed. These unique aspects of folate binding protein suggest interesting applications for the protein as a vector for further drug and imaging agent development.     

Iron Interference in the Measurement of Selenium in Whole Blood,Plasma and Serum by Graphite Furnace Atomic Absorption

Abstract

Selenium is considered to be a trace element and the determination of diagnostic levels are most conveniently measured in blood, plasma or serum in humans and animals. The approach that is taken varies according to laboratory preferences. One such method involves the use of Graphite furance Atomic Absorption Spectroscopy (GFAAS). The simplicity of diluting the sample followed by direct determination without further preparation is the most attractive characteristic of this method, coupled with good sensitivity. Proper precautions must be taken however, including that of choosing the proper instrumental parameters for the analysis. If deuterium background correctiopn is used then then analyses should be carried out at the 204.0 nm line of Selenium. By using a matrix modifier consisting of Cu/Mg, deuterium background correction and off the wall of the graphite tube atomization, the determination of the analyte was demonstrated to be possible at the mentioned wavelength, free from iron interference present in the samples.     

光谱法研究水团簇结构对AlCl3溶液与血清白蛋白作用的影响

研究了冷冻-解冻处理对A1CI₃溶液团簇结构和AICl₃与血清白蛋白相互作用的影响。测定了AICl₃溶液冷冻-解冻处理前后电导率的变化,发现AICI₃溶液经冷冻处理后,电导率有明显增加。采用紫外分光光度法和荧光光谱法对冷冻前后AICI₃溶液与血清白蛋白相互作用的研究表明,A1C1₃溶液经冷冻-解冻处理后,与血清白蛋白的相互作用变弱,配位诱导作用降低,静态猝灭作用变小,这种相互作用变弱的效应是由于水的分子团簇结构变化引起的。     

5,7-二羟基黄酮与牛血清白蛋白相互作用的研究

用荧光光谱(FS)和紫外光谱(UV)法研究了5,7-二羟基黄酮与牛血清白蛋白之间的相互作用.实验结果表明,5,7-二羟基黄酮与BSA形成基态复合物导致内源荧光淬灭,淬灭机理主要为静态淬灭.该反应的结合常数4.16×107 L/mol,结合位点数n=1.5;并用同步荧光技术考察了5,7-二羟基黄酮对BSA构象的影响.     

酶荧光毛细分析法测定血清中微量丙酮酸

提出了一种用于血清微量丙酮酸（PA）测定的酶荧光毛细分析法（P-LE-FCA）。优选的测定条件为：乳酸脱氢酶和还原型辅酶Ⅰ的浓度分别为100U/L和60μmol/L,反应时间5min。测定PA的线性范围4—80μmol/L,检出限0.73μmol/L,RSD〈1.3%。血清共存物质对PA测定无明显干扰。使用该方法对血清PA进行测定,其回收率在93.0%—106.5%之间;结果与常规紫外分光光度法一致。本方法的样品预处理过程简单、省时,省试剂,灵敏度高,重现性好。     

人血清中几种元素的ICP－AES法测定

本文研究了应用ＩＣＰ－ＡＥＳ测定人血清中Ｃａ、Ｍｇ、Ｎａ、Ｚｎ、Ｋ、Ｐ六种元素的方法。将经前处理好的人血清中加入适当的硝酸－过氧化氢混合消解液，在消解罐中经高温、高压下，使其有效地消除血清复杂基体的干扰。选用美国ＩＣＡ９０００（Ｎ＋Ｍ）型仪器的工作条件。以国家标准物质研究中心的贮备液作标准。并采用日本人血清标准和我国ＧＢＷ０９１３１牛血清标准校准仪器。     

142名健康成人血清铜的含量测定

本文用原子吸收法对吉林市１４２名健康成人血清铜的含量进行了测定。结果表明，男性血清铜值稍代于女性，但经统计学处理无显著性差异（Ｐ＞０．０５）。提出其正常值范围。     

共振光散射法测定环境水样中痕量锡

基于在Tris-HCl介质中,痕量锡对氯酚红-人血白蛋白-十二烷基硫酸钠体系的共振散射光谱有明显的猝灭作用;考察了它们的光谱特征、影响因素和适宜的反应条件;确定了散射光强度与Sn2 的关系,从而建立了测定痕量锡的共振光散射新方法.该法在室温下进行,操作方便,灵敏度高和选择性好.其线性范围为0.2-4.0μg/L,检出限0.12μg/L,用于环境水样中痕量Sn2 的测定,相对标准偏差小于3.1%,加标回收率为95.5%-100.5%,效果良好.     

光谱法研究葛根素与牛血清白蛋白的相互作用

采用紫外、同步荧光和圆二色光谱法研究了葛根素（PUE）与牛血清白蛋白（BSA）的相互作用.紫外光谱表明,BSA在230nm和278nm处的吸收峰,随着葛根素浓度的增加而减小.同步荧光光谱表明,葛根素引起BSA中色氨酸残基所处微环境的疏水性降低.圆二色光谱表明,BSA在208nm和222nm处的负峰随着葛根素浓度的增加而增强,BSA中α-螺旋含量也随之增加.这表明葛根素与BSA的相互作用,可使蛋白质分子的疏水作用增强,导致BSA的肽链结构收缩,蛋白质的构象发生变化.