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Validation of Determination and Speciation Analysis of Selenium in Urine by HPLC and Inductively-Coupled Plasma Mass Spectrometry

机译:高效液相色谱-电感耦合等离子体质谱法测定尿液中硒含量及形态分析的验证

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摘要

The first part of this study describes determination of total Se in urine by inductively-coupled plasma mass spectrometry (ICP-MS). Determination of the most abundant Se isotope, ~(80)Se, by ICP-MS is complicated by interference of ~(40)Ar_(2). This was suppressed using a dynamic reaction cell with methane. The limit of Se detection was determined and the linearity of the obtained dependence was verified by the Mandel test. The accuracy was verified by analysis of urine with a standard Se solution. In the other part, a method for separation of selenite, selenate, selenocystine, selenomethionine and selenourea in urine was elaborated using HPLC and ICP-MS. Separation of selenate, selenomethionine, selenourea was good, but the retention times of selenite and selenocystine were very close. The optimized separation parameters were used for urine analysis in septic patients and healthy volunteer control, the food of both groups being supplemented with Se. The Se concentration in the former group was very low.
机译:本研究的第一部分描述了通过电感耦合等离子体质谱法(ICP-MS)测定尿液中的总硒。 ICP-MS测定最丰富的Se同位素〜(80)Se会受到〜(40)Ar_(2)的干扰。使用带有甲烷的动态反应池可以抑制这种情况。确定了硒的检测限,并通过Mandel检验验证了所获得依赖性的线性。通过使用标准硒溶液分析尿液来验证准确性。另一方面,使用HPLC和ICP-MS阐述了尿液中亚硒酸盐,硒酸盐,硒代半胱氨酸,硒代蛋氨酸和硒脲的分离方法。硒酸盐,硒代蛋氨酸,硒代脲的分离效果很好,但硒酸盐和硒代半胱氨酸的保留时间非常接近。优化的分离参数用于败血病患者和健康志愿者的尿液分析,两组食物均添加硒。前一组中的硒浓度非常低。

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