Comprehensive two-dimensional liquid chromatography with parallel gradients for separation of phenolic and flavone antioxidants
Comprehensive two-dimensional liquid chromatography with parallel gradients for separation of phenolic and flavone antioxidants
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DOI：
10.1016/j.chroma.2007.01.119
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发表时间：
2007-05-11
影响因子：
4.1
通讯作者：
Mondello, L.
中科院分区：
文献类型：
--
作者：
Cacciola, F.;Jandera, P.;Mondello, L.
PEG-硅胶，苯基-硅胶和C18柱的各种组合，在第一个维度上的单柱或串联（串联）排列，以及在第二维度上的整体Chromolith柱进行了测试，用于全面的二维（2D）LC x LC分离酚类和黄酮类天然抗氧化剂。不同固定相化学的组合提供了第一维和第二维分离系统之间的低选择性相关性。通过在整个2D分离时间范围内使用具有在二维中平行运行的匹配轮廓的梯度，实现了系统正交性、带宽抑制、在整个2D保留平面上更规则的频带分布以及在不同2D设置中增加的峰值容量的改善。代替两个采样环，使用两个交替捕获XTerra柱将样品级分从第一维柱转移到第二维。与第一维度的PEG-二氧化硅或苯基-二氧化硅柱相比，XTerra柱上的保留更强，允许将样品馏分聚焦在捕获柱顶部的狭窄区域中，并以非常低的体积反冲洗到第二维度的移动的相。这种分数传输调制在第二维中提供了显著的带宽抑制。采用优化的固定相选择性、平行梯度和级分转移调制的二维系统，使用两个捕集柱，用于分析啤酒和葡萄酒样品中的天然抗氧化剂。(c)2007 Elsevier B. V.保留所有权利。
Various combinations of PEG-silica, phenyl-silica and C18 columns in a single-column or serial (tandem) arrangement in the first dimension and a monolithic Chromolith column in the second dimension were tested for comprehensive two-dimensional (2D) LC x LC separation of phenolic and flavone natural antioxidants. The combinations of different stationary phase chemistries provided low selectivity correlations between the first-dimension and the second-dimension separation systems. Improvement in system orthogonality, bandwidths suppression, more regular band distribution over the whole 2D retention plane and increased peak capacity in different 2D setups was achieved by using gradients with matching profiles running in parallel in the two dimensions over the whole 2D separation time range. Instead of two sampling loops, two alternating trapping XTerra columns were used for sample fraction transfer from the first-dimension column to the second dimension. Stronger retention on the XTerra columns in comparison to PEG-silica or phenyl-silica columns in the first dimension allowed using focusing of sample fractions in narrow zones on the top of a trapping column and back-flushing into the second dimension in a very low volume of the mobile phase. This fraction transfer modulation provided significant bandwidth suppression in the second dimension. 2D systems with optimized stationary phase selectivity, parallel gradients and fraction transfer modulation using two trapping columns were applied for the analysis of natural antioxidants in beer and wine samples. (c) 2007 Elsevier B.V. All rights reserved.