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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >DETERMINATION OF THIOCYANATE, IODIDE, NITRATE AND NITRITE IN BIOLOGICAL SAMPLES BY MICELLAR ELECTROKINETIC CAPILLARY CHROMATOGRAPHY
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DETERMINATION OF THIOCYANATE, IODIDE, NITRATE AND NITRITE IN BIOLOGICAL SAMPLES BY MICELLAR ELECTROKINETIC CAPILLARY CHROMATOGRAPHY

机译：胶束电动毛细管色谱法测定生物样品中的硫氰酸根，碘根，硝酸根和亚硝酸根

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Micellar electrokinetic capillary chromatography (MECC) has been developed as an efficient method for the determination of the thiocyanate ion, iodide, nitrite and nitrate. The use of various alkyltrimethylammonium ions was found advantageous for MECC compared to negatively charged surfactants, as this resulted in low migration times for the anions and thereby fast analysis. Moreover, the MECC system, using positively charged surfactants (dodecyltrimethylammonium bromide, DTAB), was effective in separating the anions of interest from interfering organic anions present in extracts from biological samples such as milk and blood. Detection of the anions was performed by direct UV. The performance of the developed method was satisfying; however, a low number of theoretical plates for the thiocyanate ion indicated the need for some improvements in this respect. The sensitivity of the method increased with a factor two by using a 75 mu m I.D. capillary instead of the 50 mu m I.D. capillary, whereas use of a high-sensitivity optical cell assembly increased the sensitivity an additional nine times. Repeatability with the 50-mu m capillary was satisfying with respect to migration time, relative migration time and normalised peak area (except for the thiocyanate ion) of the anions, with relative standard deviations varying between 0.24 and 0.29%, 0.07 and 0.16%, and 1.75 and 2.37%, respectively, whereas some improvements are still needed for the normalised and relative normalised peak areas for the thiocyanate ion (13.50 and 13.91%). Apart from the thiocyanate ion (r(2) = 0.9748), linearity studies gave correlation coefficients between 0.9962 and 0.9975 for the normalised peak areas.
机译：已开发出胶束电动毛细管色谱法（MECC）作为测定硫氰酸根离子，碘离子，亚硝酸根和硝酸根的有效方法。与带负电荷的表面活性剂相比，发现使用各种烷基三甲基铵离子对MECC有利，因为这导致阴离子的迁移时间很短，从而可以快速分析。此外，使用带正电荷的表面活性剂（十二烷基三甲基溴化铵，DTAB）的MECC系统可有效地将目标阴离子与存在于生物样品（如牛奶和血液）提取物中的干扰有机阴离子分离。通过直接UV检测阴离子。所开发方法的性能令人满意。然而，硫氰酸根离子的理论塔板数很少，表明在这方面需要一些改进。通过使用75微米的内径，该方法的灵敏度提高了两倍。毛细管而不是50微米内径毛细管，而使用高灵敏度的光学电池组件将灵敏度又提高了九倍。在阴离子的迁移时间，相对迁移时间和归一化峰面积（硫氰酸根离子除外）方面，使用50微米毛细管的重复性令人满意，相对标准偏差在0.24和0.29％，0.07和0.16％之间，分别为1.75和2.37％，而硫氰酸根离子的归一化峰面积和相对归一化峰面积（13.50和13.91％）仍需要改进。除了硫氰酸根离子（r（2）= 0.9748），线性研究得出的归一化峰面积的相关系数在0.9962和0.9975之间。

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