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Application of fractionized sampling and stacking for construction of an interface for online heart-cutting two-dimensional liquid chromatography

机译:分次采样和叠加在构建心切二维液相色谱在线界面中的应用

摘要

In this study, an efficient interface, based on a fractionized sampling and stacking (FSS) strategy, was developed for online heart-cutting two-dimensional liquid chromatography (2D LC). This interface consisted of a two-position 4-port valve, a two-position 6-port valve and a two-position 10-port valve equipped with two 450-mu L stainless steel loops. Hydrophilic interaction chromatography (HILIC) and reversed phase liquid chromatography (RP LC) were used in the first and second dimensions, respectively. The peak compression efficiency of this interface was investigated by analysis of ten standards. Good peak shapes of the ten standards were observed when the dilution ratio was over five and the co-eluate plug volume was less than 10 mu L The 2D LC system was further applied to analysis of a crude extract of Panax ginseng leaves. Seventeen major constituents in the extract were monitored, which could not be well separated by one-dimensional (1D) HILIC or RP LC method in a long separation gradient. The FSS interface successfully achieved the efficient combination of HILIC and RP LC, and the 17 constituents in ginseng extract got well separated under the optimized conditions. The FSS interface has shown great potential for 2D LC analysis of complex natural product samples. (C) 2016 Published by Elsevier B.V.
机译:在这项研究中,开发了一种基于分份采样和堆叠(FSS)策略的有效接口,用于在线心脏切割二维液相色谱(2D LC)。该接口包括一个两位四通阀,一个两位六通阀和一个两位10通阀,配有两个450μL不锈钢环路。在第一维和第二维中分别使用了亲水相互作用色谱(HILIC)和反相液相色谱(RP LC)。通过分析十种标准液,研究了该界面的峰值压缩效率。当稀释比例超过5且共洗脱液塞子体积小于10μL时,观察到10个标准品的峰形良好。2D LC系统进一步用于分析人参叶片的粗提物。监测了提取物中的17种主要成分,这些成分在长分离梯度下无法通过一维(1D)HILIC或RP LC方法很好地分离。 FSS接口成功实现了HILIC和RP LC的有效结合,在最佳条件下人参提取物中的17种成分得到了很好的分离。 FSS界面显示了对复杂天然产物样品进行二维液相色谱分析的巨大潜力。 (C)2016由Elsevier B.V.发布

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