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Authors: Jonathan BissonORCID , Marion Brunel, Alain Badoc, Grégory Da Costa, Tristan Richard, Jean-Michel Mérillon, Pierre Waffo-Téguo
Journal: Analytical Chemistry (RoMEO status: White)
Subjects: Analytical Chemistry Preparative chemistry Reverse engineering Hyphenation CPC NMR SPE
Centrifugal partition chromatography (CPC) and all countercurrent separation apparatus provide chemists with efficient ways to work with complex matrixes, especially in the domain of natural products. However, despite the great advances provided by these techniques, more efficient ways of analyzing the output flow would bring further enhancement. This study describe a hyphenated approach made by coupling NMR with CPC through a hybrid-indirect coupling made possible by using a solid phase extraction (SPE) apparatus intended for high-pressure liquid chromatography (HPLC)-NMR hyphenation.
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Authors: Alison D. Pawlus, Emma Cantos-Villar, Tristan Richard, Jonathan BissonORCID , Pascal Poupard, Yorgos Papastamoulis, Jean-Pierre Monti, Pierre-Louis Teissedre, Pierre Waffo-Téguo, Jean-Michel Mérillon
Journal: Journal of Chromatography A (RoMEO status: Green)
Subjects: Analytical Chemistry Dereplication LC-NMR Vine Wine
Wine is a major dietary source of numerous potentially health promoting stilbenoids that have been the subject of many qualitative and quantitative studies. However, our initial HPLC–MS analyses of crude wine samples demonstrated the presence of compounds with molecular weights matching characteristic stilbenoid dimers, trimers, and tetramers that were unaccounted for in the literature. Due to the likelihood that these are known compounds, a chemical dereplication method is highly desirable. We developed such a method using LC-DAD–MS monitored fractionation steps, using adsorption and centrifugal partition chromatography (CPC), to obtain fractions rich in stilbenoids for analysis in stopped-flow LC–NMR.
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# Conferences/

Hyphenating countercurrent chromatography with NMR and mass spectrometry. How to enhance the range of the liquid phases

Countercurrent chromatography techniques are increasingly used in the fractionation and purification steps of natural products due to their excellent versatility and efficiency. However, one of the major bottlenecks in liquid-liquid chromatography is the solvent system selection. In this work, a NMR-based analysis of complex solvent mixtures was developed for biphasic system selection and modification. This allowed us to develop more versatile separation conditions, such as gradients. Additionally, we hyphenated our countercurrent chromatography device with NMR and mass spectrometry.
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Authors: Jonathan BissonORCID , Pascal Poupard, Alison D. Pawlus, Alexandre Pons, Philippe Darriet, Jean-Michel Mérillon, Pierre Waffo-Téguo
Journal: Journal of Chromatography A (RoMEO status: Green)
Subjects: Analytical Chemistry Preparative chemistry Hyphenation CPC MS back-step Vine Wine
The phytochemical study of the root extract of the stilbenoid-rich Vitis riparia × Vitis berlandieri grapevine was carried out by centrifugal partition chromatography (CPC). For this reason, we developed a new elution mode we named back-step, which allowed us to obtain cleaner fractions and a more efficient separation process when used in conjunction with a classical elution approach. Three hydroxystilbenes: (E)-resveratrol, (E)-ɛ-viniferin and (E)-vitisin C, with greater than 90% purity were thus obtained through such process, with minimal sample handling and purification steps.
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