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Continuous vs. segmented second-dimension system gradients for comprehensive two-dimensional liquid chromatography of sugarcane (Saccharum spp.)

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Abstract

A comprehensive two-dimensional liquid chromatography system in combination with photodiode array and mass spectrometry detection was developed for analysis of polyphenols in sugarcane (Saccharum spp.) leaf extracts. To achieve this, a micro cyano column and a partially porous octodecylsilica column were used in the first and the second dimension, respectively. The choice of the cyano column over other reversed-phase columns tested for the first-dimension separation was due to its lower correlation selectivity with respect to the octodecylsilica column, which was used for the second-dimension separation. Even when reversed-phase mode was used in both dimensions, a satisfactory degree of orthogonality was achieved by use of different gradient elution modes in the second dimension. By means of the setup investigated, 38 polyphenolic compounds were detected, and among them 24 were positively identified by means of complementary data from photodiode array and mass spectrometry detection and an in-house database. This is the first time such a powerful analytical technique has been used for polyphenolic characterization of sugarcane extracts.

RP-LC×RP-LC contour plot of a sugarcane leaf extract

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Acknowledgments

The authors gratefully acknowledge Shimadzu and Sigma-Aldrich/Supelco for their continuous support. G.M.L. thanks the Conselho Nacional de Desenvolvimento Científico e Tecnológico for a scholarship (process number BEX 5605/13-0).

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Authors and Affiliations

  1. Dipartimento di Scienze del Farmaco e dei Prodotti per la Salute, University of Messina, Viale Annunziata, 98168, Messina, Italy

    Gabriel Mazzi Leme, Paola Donato, Paola Dugo & Luigi Mondello

  2. Institute of Chemistry, São Paulo State University - UNESP, Rua Prof. Francisco Degni 55, Araraquara, SP, 14800-06, Brazil

    Gabriel Mazzi Leme & Alberto José Cavalheiro

  3. Dipartimento di Scienze dell’Ambiente, della Sicurezza, del Territorio, degli Alimenti e della Salute, University of Messina, Viale F. Stagno d’Alcontres 31, 98166, Messina, Italy

    Francesco Cacciola

  4. Chromaleont s.r.l. A start-up of the University of Messina, c/o Dipartimento di Scienze del Farmaco e dei Prodotti per la Salute, University of Messina, Viale Annunziata, 98168, Messina, Italy

    Francesco Cacciola, Paola Donato, Paola Dugo & Luigi Mondello

  5. Centro Integrato di Ricerca, University Campus Bio-Medico of Rome, Via Álvaro del Portillo 21, 00128, Rome, Italy

    Paola Donato, Paola Dugo & Luigi Mondello

Authors
  1. Gabriel Mazzi Leme
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  2. Francesco Cacciola
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  3. Paola Donato
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  4. Alberto José Cavalheiro
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  5. Paola Dugo
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  6. Luigi Mondello
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Corresponding author

Correspondence to Luigi Mondello.

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Leme, G.M., Cacciola, F., Donato, P. et al. Continuous vs. segmented second-dimension system gradients for comprehensive two-dimensional liquid chromatography of sugarcane (Saccharum spp.). Anal Bioanal Chem 406, 4315–4324 (2014). https://doi.org/10.1007/s00216-014-7786-8

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  • DOI: https://doi.org/10.1007/s00216-014-7786-8

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