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首页> 外文期刊>Journal of separation science. >Multidimensional LC x LC analysis of phenolic and flavone natural antioxidants with UV-electrochemical coulometric and MS detection
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Multidimensional LC x LC analysis of phenolic and flavone natural antioxidants with UV-electrochemical coulometric and MS detection

机译：紫外-电化学库仑法和MS检测对酚类和黄酮类天然抗氧化剂的多维LC x LC分析

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摘要

A comprehensive 2-D LC x LC system was developed for the separation of phenolic and flavone antioxidants, using a PEG-silica column in the first dimension and a C-18 column with porous-shell particles or a monolithic column in the second dimension. Combination of PEG and C18 or C8 stationary phase chemistries provide low selectivity correlations between the first dimension and the second dimension separation systems. This was evidenced by large differences in structural contributions to the retention by -CCOH, -OH and other substituents on the basic phenol or flavone structure. Superficially porous columns with fused core particles or monolithic columns improve the resolution and speed of second dimension separation in comparison to a fully porous particle C18 column. Increased peak capacity and high orthogonality in different 2-D setups was achieved by using gradients with matching profiles running in parallel in the two dimensions over the whole 2-D separation time range. Multi-dimensional set-up combining the LC x LC separation on-line with UV and multi-channel coulometric detection and off-line with MS/MS technique allowed positive peak identification. The Coularray software compensates for the effects of the baseline drift during the gradient elution and is compatible with parallel gradient comprehensive LC x LC technique. Furthermore, it provides significant improvement in the sensitivity and selectivity of detection in comparison to both UV and MS detection. The utility of these systems has been demonstrated in the analysis of beer samples.
机译：开发了一种全面的二维LC x LC系统，用于分离酚类和黄酮类抗氧化剂，使用一维的PEG硅胶柱和二维的带有多孔壳颗粒的C-18柱或整体柱。 PEG与C18或C8固定相化学试剂的组合在第一维和第二维分离系统之间提供了低选择性相关性。这通过在基本酚或黄酮结构上对-CCOH，-OH和其他取代基的保留贡献的结构差异很大而得到证明。与完全多孔的颗粒C18色谱柱相比，具有熔融核芯颗粒或整体柱的表面多孔色谱柱提高了二维分离的分离度和速度。通过使用在整个二维分离时间范围内在二维中平行运行的匹配轮廓的梯度，可以在不同的二维设置中提高峰容量和高正交性。多维设置将LC x LC分离在线与UV和多通道库仑检测相结合，以及离线与MS / MS技术相结合，可实现正峰鉴定。 Coularray软件补偿了梯度洗脱过程中基线漂移的影响，并且与并行梯度综合LC x LC技术兼容。此外，与UV和MS检测相比，它在检测的灵敏度和选择性方面提供了显着的提高。这些系统的实用性已在啤酒样品分析中得到证明。

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