分段富集中心切割二维液相色谱接口技术在中药大黄分析中的应用

【作者】 季宝成； 马风伟； 夏兵； 周燕；

【机构】 中国科学院成都生物研究所；

【摘要】 <正>随着生命科学、材料科学和环境科学等的发展,复杂样品体系的分离分析成为分析化学的重要研究方向。自20世纪70年代以来,无论在色谱基础理论,还是在仪器性能方面都得到了很大程度的完善和提高。尽管色谱填料粒径的降低和固定相表面理化特性的改进极大地提高了液相色谱柱分辨能力,但是液相色谱真正的分离能力却没有能够随之显著提°?ú更多还原

【Abstract】 Inthis study,a novel and efficient interface for online stop-flow twodimensionalultra-high performance liquid chromatographic(2 DUPLC) system was developed based on a fractionized sampling and stacking(FSS) strategy.This interface consists of a two-position 4-port valve,a two-position 6-port valve and a two-position 10-port valve equipped with two 450 μL stainless steel loops.Hydrophilic interaction chromatography(HILIC) and reversed phase liquid chromatography(RPLC) were usedin the first and second dimension,respectively.The peak compression efficiency of this interface between two dimensionswas evaluated by analysis of ten standard compounds.Good peak shapes for ten standards were acquired when the dilution ratio was set over 5.The 2 DUPLC system was further applied to analyze the crude extracts of Rheum palmatum L.Under an optimized condition,most of the compounds in the extracts of R.palmatumwere well separated and a total of seventeenconstituents were tentatively identified by coupling the system with tandem mass spectrometry(MS/MS),which showedgood application prospect in the analysis of complex matrix samples such as traditional Chinese medicines(TCMs).更多还原