Hyphenating Centrifugal Partition Chromatography with Nuclear Magnetic Resonance through Automated Solid Phase Extraction.
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. Some hardware changes were needed to adapt the incompatible flow-rates and a reverse-engineering approach that led to the specific software required to control the apparatus. 1D1HNMR and1H-1H correlation spectroscopy (COSY) spectra were acquired in reasonable time without the need for any solvent-suppression method thanks to the SPE nitrogen drying step. The reduced usage of expensive deuterated solvents from several hundreds of milliliters to the milliliter order is the major improvement of this approach compared to the previously published ones.
Université Bordeaux , Faculté des Sciences Pharmaceutiques, ISVV, EA 4577 Œnologie, Molécules d'Intérêt Biologique (GESVAB), F-33882 Villenave-d'Ornon, France.
Jonathan
J
Bisson
Université Bordeaux , Faculté des Sciences Pharmaceutiques, ISVV, EA 4577 Œnologie, Molécules d'Intérêt Biologique (GESVAB), F-33882 Villenave-d'Ornon, France.
Marion
M
Brunel
Université Bordeaux , Faculté des Sciences Pharmaceutiques, ISVV, EA 4577 Œnologie, Molécules d'Intérêt Biologique (GESVAB), F-33882 Villenave-d'Ornon, France.|INRA, ISVV, USC 1366 Œnologie, F-33882 Villenave-d'Ornon, France.
Alain
A
Badoc
Université Bordeaux , Faculté des Sciences Pharmaceutiques, ISVV, EA 4577 Œnologie, Molécules d'Intérêt Biologique (GESVAB), F-33882 Villenave-d'Ornon, France.|INRA, ISVV, USC 1366 Œnologie, F-33882 Villenave-d'Ornon, France.
Grégory
G
Da Costa
Université Bordeaux , Faculté des Sciences Pharmaceutiques, ISVV, EA 4577 Œnologie, Molécules d'Intérêt Biologique (GESVAB), F-33882 Villenave-d'Ornon, France.|INRA, ISVV, USC 1366 Œnologie, F-33882 Villenave-d'Ornon, France.
Tristan
T
Richard
Université Bordeaux , Faculté des Sciences Pharmaceutiques, ISVV, EA 4577 Œnologie, Molécules d'Intérêt Biologique (GESVAB), F-33882 Villenave-d'Ornon, France.|INRA, ISVV, USC 1366 Œnologie, F-33882 Villenave-d'Ornon, France.
Jean-Michel
JM
Mérillon
Université Bordeaux , Faculté des Sciences Pharmaceutiques, ISVV, EA 4577 Œnologie, Molécules d'Intérêt Biologique (GESVAB), F-33882 Villenave-d'Ornon, France.|INRA, ISVV, USC 1366 Œnologie, F-33882 Villenave-d'Ornon, France.
Pierre
P
Waffo-Téguo