Cpc

# Publications/

Hyphenating Centrifugal Partition Chromatography with Nuclear Magnetic Resonance through Automated Solid Phase Extraction

Journal: Analytical Chemistry (RoMEO status: White) Published on
Categories: publications
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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# Publications/

New E-miyabenol isomer isolated from grapevine cane using centrifugal partition chromatography guided by mass spectrometry

Journal: Tetrahedron (RoMEO status: Green) Published on
Categories: publications
Subjects: Pharmacognosy Phytochemistry Vine Wine Stilbenoids Polyphenols CPC Mass Spectrometry

Stilbenoids have received increasing attention over the last two decades since the discovery of resveratrol in wine. With an ever-growing rhythm, a multitude of biological activities of naturally occurring stilbenes are being reported. In this work, we investigated minor stilbenoid compounds from Vitis vinifera stalks. The compounds were purified by means of centrifugal partition chromatography (CPC), a countercurrent-separation technique. Electrospray ionization–ion trap mass spectrometry (ESI–IT-MS) after optimization proved to be extremely efficient for the detection of these new molecules, providing both structural information for structure elucidation and a means to achieve identification even with minute amounts.

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# Publications/

Centrifugal partition chromatography applied to the isolation of oak wood aroma precursors

Journal: Food Chemistry (RoMEO status: Green) Published on
Categories: publications
Subjects: CPC Oak Wood Flavor Wine

Flavours extracted from oak wood during barrel ageing contribute to the organoleptic character of wines and spirits. The aim of this work was to identify the glycosidic precursors of the key volatile compounds responsible for oak wood aroma. Oak extract is a very complex matrix and, furthermore, precursors are present in very small quantities. Preparative centrifugal partition chromatography (CPC) is a promising solution for purifying the oak extract. The solvent system was selected on the basis of the partition coefficient of glycosidase enzyme activity (Kca).

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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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# Publications/

Development of hybrid elution systems for efficient purification of stilbenoids using centrifugal partition chromatography coupled to mass spectrometry

Journal: Journal of Chromatography A (RoMEO status: Green) Published on
Categories: publications
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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