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Supercritical Fluid Chromatography × Ultra-High Pressure Liquid Chromatography for Red Chilli Pepper Fingerprinting by Photodiode Array, Quadrupole-Time-of-Flight and Ion Mobility Mass Spectrometry (SFC × RP-UHPLC-PDA-Q-ToF MS-IMS)

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Abstract

The coupling of normal phase and reversed phase liquid chromatography (NP-LC × RP-LC) is one of the most effective ways to increase orthogonality in two-dimensional comprehensive separations, being the two retention mechanisms truly independent. However, such coupling is not straightforward to implement, due to immiscibility of the mobile phases, poor peak focusing at the head of the secondary column (2D), signal interferences and peak deterioration. In this research, supercritical fluid chromatography (SFC) was used in the first dimension (1D), coupled to ultra high pressure LC (UHPLC), to alleviate incompatibility issues and provide a number of advantages related to the use of supercritical CO2. An on-line SFC × RP-UHPLC system was implemented in an automated fashion, around two 2-position, six-port switching valves equipped with octadecyl silica cartridges for effective trapping and focusing of the analytes eluted from 1D. A water make-up flow added to the SFC effluent permitted to efficiently focus the solutes on the sorbent material and to reduce interferences of the expanded CO2 on the 2D separation. In addition to photodiode array and quadrupole-time-of-flight mass spectrometry detection, ion mobility separation based on analyte mass, shape and size added a fourth separation dimension for carotenoid fingerprinting in a red chilli pepper sample.

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Acknowledgements

The authors gratefully acknowledge Waters and Millipore Sigma/Supelco Corporations for their continuous support.

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Authors and Affiliations

  1. Dipartimento di Scienze Biomediche, Odontoiatriche e delle Immagini Morfologiche e Funzionali, University of Messina, via Consolare Valeria, 98125, Messina, Italy

    Paola Donato & Daniele Giuffrida

  2. Dipartimento di Scienze Chimiche, Biologiche, Farmaceutiche ed Ambientali, University of Messina - Polo Annunziata, Viale Annunziata, 98168, Messina, Italy

    Marianna Oteri, Veronica Inferrera, Paola Dugo & Luigi Mondello

  3. Centro Integrato di Ricerca (C.I.R.), University Campus Bio-Medico of Rome, Via Álvaro del Portillo 21, 00128, Rome, Italy

    Paola Dugo & Luigi Mondello

  4. Chromaleont S.r.l., via Leonardo Sciascia Coop. Fede, Pal. B, 98168, Messina, Italy

    Paola Dugo & Luigi Mondello

Authors
  1. Paola Donato
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  2. Daniele Giuffrida
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  3. Marianna Oteri
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  4. Veronica Inferrera
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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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This article does not contain any studies with human participants or animals performed by any of the authors.

Conflict of Interest

Paola Donato declares that she has no conflict of interest. Daniele Giuffrida declares that he has no conflict of interest. Marianna Oteri declares that she has no conflict of interest. Veronica Inferrera declares that she has no conflict of interest. Paola Dugo declares that she has no conflict of interest. Luigi Mondello declares that he has no conflict of interest.

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Donato, P., Giuffrida, D., Oteri, M. et al. Supercritical Fluid Chromatography × Ultra-High Pressure Liquid Chromatography for Red Chilli Pepper Fingerprinting by Photodiode Array, Quadrupole-Time-of-Flight and Ion Mobility Mass Spectrometry (SFC × RP-UHPLC-PDA-Q-ToF MS-IMS). Food Anal. Methods 11, 3331–3341 (2018). https://doi.org/10.1007/s12161-018-1307-x

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  • DOI: https://doi.org/10.1007/s12161-018-1307-x

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