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Characterization of grape seed procyanidins by comprehensive two-dimensional hydrophilic interaction × reversed phase liquid chromatography coupled to diode array detection and tandem mass spectrometry

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Abstract

In this work, the development and optimization of a new methodology to analyze grape seed procyanidins based on the application of two-dimensional comprehensive LC is presented. This two-dimensional method involves the use of a microbore column containing a diol stationary phase in the first dimension coupled to either a C18 partially porous short column or a C18 monolithic column in the second dimension. The orthogonal hydrophilic interaction × reversed phase liquid chromatography (HILIC×RP-LC) system is interfaced through a ten-port two-position switching valve. The optimized HILIC×RP-LC separation followed by diode array and tandem mass spectrometry detection (HILIC×RP-LC-DAD-MS/MS) made possible the direct analysis of a complex grape seed extract and allowed the tentative identification of 43 flavan-3-ols, including monomers and procyanidin oligomers till a polymerization degree of 7 units with different galloylation degrees. To the best of our knowledge, this is the first time that this powerful analytical technique is employed to characterize complex procyanidin samples. This work successfully demonstrates the great capabilities of the HILIC×RP-LC-DAD-MS/MS coupling for the direct analysis of very complex natural samples like grape seeds.

Two-dimensional HILIC x RP plot (280 nm) of grape seed procyanidins.

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Acknowledgments

M.H. would like to thank MICINN for his “Ramón y Cajal” research contract. The authors want to thank Projects AGL2011-29857-C03-01 and CONSOLIDER INGENIO 2010 CSD2007-00063 FUN-C-FOOD (Ministerio de Educación y Ciencia) for the financial support.

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Authors and Affiliations

  1. Laboratory of Foodomics, Institute of Food Science Research (CIAL, CSIC-UAM), Nicolás Cabrera 9, Campus Cantoblanco, 28049, Madrid, Spain

    Lidia Montero, Miguel Herrero, Elena Ibáñez & Alejandro Cifuentes

  2. Department of Production and Characterization of Novel Foods, Institute of Food Science Research (CIAL, CSIC-UAM), Nicolás Cabrera 9, Campus Cantoblanco, 28049, Madrid, Spain

    Marin Prodanov

Authors
  1. Lidia Montero
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  2. Miguel Herrero
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  3. Marin Prodanov
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  4. Elena Ibáñez
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  5. Alejandro Cifuentes
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Correspondence to Miguel Herrero.

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Published in the topical collection Nutraceuticals and Separations with guest editor Luigi Mondello.

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Montero, L., Herrero, M., Prodanov, M. et al. Characterization of grape seed procyanidins by comprehensive two-dimensional hydrophilic interaction × reversed phase liquid chromatography coupled to diode array detection and tandem mass spectrometry. Anal Bioanal Chem 405, 4627–4638 (2013). https://doi.org/10.1007/s00216-012-6567-5

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  • DOI: https://doi.org/10.1007/s00216-012-6567-5

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