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Ionic liquid capillary columns for analysis of multi-component volatiles by gas chromatography-mass spectrometry: performance, selectivity, activity and retention indices

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Abstract

This study investigates applications and performance evaluation of SLB-IL60, SLB-IL76 and SLB-IL111 columns, in relation to a DB-Wax column, for the analysis of coffee volatile compounds. Both standards and an authentic coffee sample were analysed, with solid-phase microextraction (SPME) sampling of the latter. A cryofocusing method was applied to improve resolution of the earliest eluting peaks using splitless injection SPME sample analysis. The Grob test was used to verify the inertness and efficiency of the columns, helping to understand the interactions between analytes and stationary phases, particularly toward more polar coffee analytes. A DB-5 column was used only in analysis of n-alkanes and Grob test mixtures as an apolar reference. The evaluated ionic liquid columns showed a moderate acid-base character and low inertness for compounds with hydrogen bond capabilities, especially for the hydroxylated analytes, 2,3-butanediol in the Grob test, and furanones and acids in the coffee standards. The columns exhibiting the best resolution and efficiency were DB-Wax and SLB-IL60, both for samples and standards. Although the DB-Wax column is preferred for analysis of coffee volatiles, due to better inertness, the evaluated ionic liquid columns allowed identification of compounds that were not observed in separations with the Wax-phase column in this work. Among these compounds is 3,4-dimethyl-2,5-furandione, seldom reported in the literature of coffee. Proposed improvement by the manufacturer in the inertness of the columns evaluated in this study may lead to better results; so future versions of IL phases may be better applied in the separation of target analytes, especially those with basic character.

Illustrative representation of the sample (coffee) and the chemical structures of the stationary phases of the ionic liquid capillary columns used as object of study in the present work.

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Acknowledgments

The authors thank collaborating researchers from Universidade Federal do Rio de Janeiro (UFRJ) and Embrapa Agroindústria de Alimentos who assisted with this study. We also thank the financial support of Brazilian agencies Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES), Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) and Fundação Carlos Chagas Filho de Amparo à Pesquisa do Estado do Rio de Janeiro (FAPERJ).

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Authors and Affiliations

  1. Instituto de Química, Universidade Federal do Rio de Janeiro (UFRJ), Rio de Janeiro, 21945-970, Brazil

    Michelle S. S. Amaral & Claudia M. Rezende

  2. School of Chemistry, Monash University, Wellington Road, Clayton, Victoria, 3800, Australia

    Philip J. Marriott

  3. Embrapa Agroindústria de Alimentos, Av. das Américas, 29501, Rio de Janeiro, 23020-470, Brazil

    Humberto R. Bizzo

Authors
  1. Michelle S. S. Amaral
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  2. Philip J. Marriott
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  3. Humberto R. Bizzo
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  4. Claudia M. Rezende
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Correspondence to Philip J. Marriott or Claudia M. Rezende.

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The authors declare that they have no conflicts of interest.

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Published in the topical collection Ionic Liquids as Tunable Materials in (Bio)Analytical Chemistry with guest editors Jared L. Anderson and Kevin D. Clark.

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Amaral, M.S.S., Marriott, P.J., Bizzo, H.R. et al. Ionic liquid capillary columns for analysis of multi-component volatiles by gas chromatography-mass spectrometry: performance, selectivity, activity and retention indices. Anal Bioanal Chem 410, 4615–4632 (2018). https://doi.org/10.1007/s00216-017-0718-7

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  • DOI: https://doi.org/10.1007/s00216-017-0718-7

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