Untargeted profiling of Glycyrrhiza glabra extract with comprehensive two-dimensional liquid chromatography-mass spectrometry using multi-segmented shift gradients in the second dimension: Expanding the metabolic coverage

Yong Foo Wong, Francesco Cacciola, Soraya Fermas, Solange Riga, Darryl James, Valeria Manzin, Brice Bonnet, Philip John Marriott, Paola Dugo, Luigi Mondello

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5 Citations (Scopus)

Abstract

Metabolic profiling of Glycyrrhiza glabra using comprehensive two-dimensional liquid chromatography (LC × LC) coupled with photodiode array (PDA) and mass spectrometry (MS) detection is described. The separation was conducted under reversed-phase conditions, using a combination of first dimension (1D) 150 mm microbore cyano column utilising 2.7 μm diameter (dp) particles, and second dimension (2D) 50 mm superficially porous octadecylsilica column with 2.7 μm dp particles. A multi-segmented shift gradient (MSG) for the 2D separation was developed, and the orthogonality achieved was compared with other modes of gradients, such as full in-fraction, and shift gradient systems. Results demonstrated a significant expansion of metabolic coverage using MSG in 2D, providing the highest measure of orthogonality compared to other gradient modes. Compound identifications were performed by employing complementary data from PDA and MS detection, with reference to structural group-type distribution in 2D space. A total of ca. 120 compounds were detected, and among them 37 were tentatively identified, distributed over the chemical families of glycosylated flavanones, triterpene saponins, and others. In comparison with one-dimensional LC, the total number of compounds detected was ca. 2-fold greater when LC × LC was employed. To the best of our knowledge, this is the first demonstration of the MSG mode in LC × LC, representing a powerful strategy to expand the metabolic coverage for analysis of plant-derived extracts, containing a multitude of different phytochemical classes.

Original languageEnglish
Pages (from-to)1993-2000
Number of pages8
JournalElectrophoresis
Volume39
Issue number15
DOIs
Publication statusPublished - 2018

Keywords

  • Flavanones
  • LC×LC-PDA-MS
  • Licorice
  • Metabolic coverage
  • Orthogonality
  • Plant extracts

Cite this

Wong, Yong Foo ; Cacciola, Francesco ; Fermas, Soraya ; Riga, Solange ; James, Darryl ; Manzin, Valeria ; Bonnet, Brice ; Marriott, Philip John ; Dugo, Paola ; Mondello, Luigi. / Untargeted profiling of Glycyrrhiza glabra extract with comprehensive two-dimensional liquid chromatography-mass spectrometry using multi-segmented shift gradients in the second dimension : Expanding the metabolic coverage. In: Electrophoresis. 2018 ; Vol. 39, No. 15. pp. 1993-2000.
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abstract = "Metabolic profiling of Glycyrrhiza glabra using comprehensive two-dimensional liquid chromatography (LC × LC) coupled with photodiode array (PDA) and mass spectrometry (MS) detection is described. The separation was conducted under reversed-phase conditions, using a combination of first dimension (1D) 150 mm microbore cyano column utilising 2.7 μm diameter (dp) particles, and second dimension (2D) 50 mm superficially porous octadecylsilica column with 2.7 μm dp particles. A multi-segmented shift gradient (MSG) for the 2D separation was developed, and the orthogonality achieved was compared with other modes of gradients, such as full in-fraction, and shift gradient systems. Results demonstrated a significant expansion of metabolic coverage using MSG in 2D, providing the highest measure of orthogonality compared to other gradient modes. Compound identifications were performed by employing complementary data from PDA and MS detection, with reference to structural group-type distribution in 2D space. A total of ca. 120 compounds were detected, and among them 37 were tentatively identified, distributed over the chemical families of glycosylated flavanones, triterpene saponins, and others. In comparison with one-dimensional LC, the total number of compounds detected was ca. 2-fold greater when LC × LC was employed. To the best of our knowledge, this is the first demonstration of the MSG mode in LC × LC, representing a powerful strategy to expand the metabolic coverage for analysis of plant-derived extracts, containing a multitude of different phytochemical classes.",
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Untargeted profiling of Glycyrrhiza glabra extract with comprehensive two-dimensional liquid chromatography-mass spectrometry using multi-segmented shift gradients in the second dimension : Expanding the metabolic coverage. / Wong, Yong Foo; Cacciola, Francesco; Fermas, Soraya; Riga, Solange; James, Darryl; Manzin, Valeria; Bonnet, Brice; Marriott, Philip John; Dugo, Paola; Mondello, Luigi.

In: Electrophoresis, Vol. 39, No. 15, 2018, p. 1993-2000.

Research output: Contribution to journalArticleResearchpeer-review

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T2 - Expanding the metabolic coverage

AU - Wong, Yong Foo

AU - Cacciola, Francesco

AU - Fermas, Soraya

AU - Riga, Solange

AU - James, Darryl

AU - Manzin, Valeria

AU - Bonnet, Brice

AU - Marriott, Philip John

AU - Dugo, Paola

AU - Mondello, Luigi

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KW - Metabolic coverage

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