Capillary zone electrophoresis of potassium in human vitreous humour: validation of a new method

Capillary zone electrophoresis of potassium in human vitreous humour: validation of a new method
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DOI:
10.1016/s0378-4347(99)00338-2
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发表时间:
1999-10-15
期刊:
JOURNAL OF CHROMATOGRAPHY B
影响因子:
--
通讯作者:
Marigo, M
Marigo, M
中科院分区:
其他
文献类型:
--
作者:
Tagliaro, F;Manetto, G;Marigo, M

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玻璃体液中钾的分析一直被认为是法医学和法医毒理学调查的重要工具,特别是用于确定死后时间。本工作旨在优化和验证一种可靠、简单和快速的毛细管电泳方法,用于人玻璃体液中钾的分析,并在214 nm波长处进行间接紫外检测。电泳分离在包含5 mM咪唑、5 mM 18-冠-6醚和6 mM D,L α-羟基丁酸(HIBA)的运行缓冲液中进行,调节至pH 4.5。通过在25 ℃下施加500 V/cm的电压进行恒定电压运行。样品以流体动力学模式在毛细管的阳极端进样(0.5 p.s.i.持续10 s; 1 p.s.i.= 6894.76帕)。该方法在6.5 mM至16.25 μ M的浓度范围内具有良好的线性关系,r(2)值为0.9994。基于信噪比为3的检测限为9.0 μ M。迁移时间的绝对日内RSD为
The analysis of potassium in the vitreous humour has long been regarded as an important tool in medicolegal and forensic toxicological investigation, particularly for the determination of the post-mortem interval. The present work was aimed at the optimisation and validation of a reliable, simple and fast capillary electrophoresis method for potassium analysis in the human vitreous humour with indirect UV detection at a wavelength of 214 nm, Electrophoretic separations were carried out in a running buffer comprising 5 mM imidazole, 5 mM 18-crown-6 ether and 6 mM D,L alpha-hydroxybutyric acid (HIBA), adjusted to pH 4.5. Constant voltage runs were carried out by applying a voltage of 500 V/cm at 25 degrees C. The samples were injected in the hydrodynamic mode at the anodic end of the capillary (0.5 p.s.i. for 10 s; 1 p.s.i.=6894.76 Pa). The method showed good linearity in the concentration range from 6.5 mM to 16.25 mu M, with an r(2) value of 0.9994. The limit of detection, based on a signal-to-noise ratio of three, was 9.0 mu M. Absolute intra-day RSDs of migration times were