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首页> 外文期刊>Journal of Pharmaceutical and Biomedical Analysis: An International Journal on All Drug-Related Topics in Pharmaceutical, Biomedical and Clinical Analysis >Optimization of a new methodology for trace determination of elements in biological fluids: Application for speciation of inorganic selenium in children's blood
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Optimization of a new methodology for trace determination of elements in biological fluids: Application for speciation of inorganic selenium in children's blood

机译:优化新方法进行痕量生物流体元素的测定方法:在儿童血液中无机硒的应用

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摘要

The continuous sample drop flow microextraction (CSDFME) joined with the iridium-modified tube graphite furnace atomic absorption spectrometry (GFAAS) has been developed as a highly sensitive technique for the speciation of selenium in blood samples. In this method 32.0 mu l carbon tetrachloride is transferred to the bottom of a conical sample cup. Then the 5.0 ml of aqueous solution transforms to fine droplets while passing through the organic solvent. At this stage, Se(IV)-APDC hydrophobic complex is extracted into the organic solvent. After extraction, the conical sample cup is transferred to the GFAAS and 20111 of extraction solvent was injected into the graphite tube by the aim of autosampler. Under the optimum conditions, the calibration graph was linear in the range of 0.06-3.0 mu gl(-1) with detection limit of 0.02 mu gl(-1).The enrichment factor and enhancement factor were 106 and 91, respectively. Repeatability (intra-day) and reproducibility (inter-day) of method based on seven replicate measurements of 2.5 mu gl(-1) of selenium were 3.7% and 4.2%, respectively. Total inorganic Se(IV, VI) was measured after reduction of Se(VI) with gentle boiling in 5 M HCI medium for 50 min and adjusting pH to 3, and the concentration of Se(VI) was calculated by subtracting the Se(IV) concentration from the total selenium concentration. (C) 2017 Elsevier B.V. All rights reserved.
机译:连续样品滴流量微萃取(CSDFME)与铱改性的管石墨炉原子吸收光谱法(GFAAS)开发为血液样品中硒形态的高敏感技术。在该方法中,将32.0μl碳四氯化碳转移到锥形样品杯的底部。然后在通过有机溶剂的同时,5.0mL水溶液转化为细液滴。在该阶段,将SE(IV)-APDC疏水复合物萃取到有机溶剂中。萃取后,通过自动进样器的目的将锥形样品杯转移到萃取溶剂的GFAAs和20111中注入石墨管中。在最佳条件下,校准图在0.06-3.0μGL(-1)的范围内,检测限为0.02μg(-1)。富集因子和增强因子分别为106和91。基于七种复制测量的硒的七次重复测量的方法的重复性(日期)和再现性分别为3.7%和4.2%。在将5M HCl培养基中的柔和沸点较低的Se(VI)还原50分钟并调节pH至3后,测量总无机SE(IV,VI),并通过减去SE(IV)来计算SE(VI)的浓度(IV )浓度从总硒浓度。 (c)2017年Elsevier B.V.保留所有权利。

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