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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Preparation of organic-inorganic hybrid silica monolith with octyl and sulfonic acid groups for capillary electrochromatograhpy and application in determination of theophylline and caffeine in beverage
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Preparation of organic-inorganic hybrid silica monolith with octyl and sulfonic acid groups for capillary electrochromatograhpy and application in determination of theophylline and caffeine in beverage

机译：毛细管电色谱法制备具有辛基和磺酸基的有机-无机杂化二氧化硅整体料及其在饮料中茶碱和咖啡因的测定中的应用

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An organic-inorganic hybrid silica monolithic column with octyl and sulfonic acid groups has been prepared by sol-gel technique for capillary electrochromatograhpy. The structure of hybrid monolith was optimized by changing the composition of tetraethoxysilane (TEOS), octyltriethoxysilane (C-8-TEOS) and 3-mercaptopropyltrimethoxysilane (MPTMS) in the mixture of precursors. Then, the obtained hybrid monolith was oxidized using hydrogen peroxide (30%, w/w) to yield sulfonic acid groups. The sulfonic acid group, which served as strong cation-exchanger, dominated the charge on the surface of the capillary column and generated stable electroosmotic flow (EOF) in a wide range of pH. The monolithic column was characterized by scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy and elemental analysis (EA), and the performance of column was evaluated in detail by separating different kinds of compounds with column efficiency up to 155,000 plates/m for thiourea. In addition, this monolithic column was also applied in the analysis of theophylline (TP) and caffeine (CA) in beverages. The detection limits were 0.39 and 0.48 mu g/mL for theophylline and caffeine, respectively. The method reproducibility was tested by evaluating the intra- and inter-clay precisions, and relative standard deviations of less than 3.9 and 8.4%. respectively, were obtained. Recoveries of compounds from spiked beverage samples ranged from 87.2 to 105.2%.
机译：通过溶胶-凝胶技术制备了具有辛基和磺酸基的有机-无机杂化硅胶整体柱，用于毛细管电色谱分析。通过改变前体混合物中的四乙氧基硅烷（TEOS），辛基三乙氧基硅烷（C-8-TEOS）和3-巯基丙基三甲氧基硅烷（MPTMS）的组成来优化杂化整体结构。然后，使用过氧化氢（30％，w​​ / w）将获得的杂化整料氧化以产生磺酸基。用作强阳离子交换剂的磺酸基支配了毛细管柱表面的电荷，并在很宽的pH范围内产生了稳定的电渗流（EOF）。通过扫描电子显微镜（SEM），傅立叶变换红外（FT-IR）光谱和元素分析（EA）对整体柱进行表征，并通过分离色谱柱效率高达155,000的各种化合物来详细评估柱的性能板/米的硫脲。此外，该整体式色谱柱还用于分析饮料中的茶碱（TP）和咖啡因（CA）。茶碱和咖啡因的检出限分别为0.39和0.48μg/ mL。通过评估粘土内部和内部的精度以及相对标准偏差小于3.9和8.4％，测试了方法的可重复性。分别获得。加标饮料样品中化合物的回收率在87.2％至105.2％之间。

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