Comprehensive two-dimensional temperature-responsive × reversed phase liquid chromatography for the analysis of wine phenolics

Wicht, Kristina; Baert, Mathijs; Muller, Magriet; Bandini, Elena; Schipperges, Sonja; Doehren, Norwin von; Desmet, Gert; Villiers, André de; Lynen, Frédéric

doi:10.1016/j.talanta.2021.122889

Cited by 21 publications

(20 citation statements)

References 68 publications

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“…To demonstrate the potential of the approach reported here to improve sensitivity for an LC × LC application, phenolic compounds extracted from blueberries were analyzed for all three column combinations with the proposed setup. The combination of TRLC and RPLC has been shown to be suitable for phenolic analysis . Hence, the combination of TRLC × RPLC-UV/MS with a narrow column in the 2 D should allow for sensitive analysis in natural product analysis to gain new insights into the identification of compounds or quantitative analysis for low abundant molecules in the future exploiting this new tool.…”

Section: Resultsmentioning

confidence: 99%

“…Due to the thermal mass of the system this process took about 15 min. It was previously found that PNIPAAm shows the lowest retention for phenolic analytes at 15 °C . The flow rates were 0.45 mL/min for the 1 mm I.D.…”

Section: Methodsmentioning

confidence: 99%

“…It was previously found that PNIPAAm shows the lowest retention for phenolic analytes at 15 °C. 28 The flow rates were 0.45 mL/ min for the 1 mm I.D. column, 1.87 mL/min for the 2.1 mm column, and 2.82 mL/min for the 3 mm column to achieve the analysis.…”

Section: ■ Experimental Sectionmentioning

confidence: 99%

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Enhanced Sensitivity in Comprehensive Liquid Chromatography: Overcoming the Dilution Problem in LC × LC via Temperature-Responsive Liquid Chromatography

et al. 2022

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In comprehensive two-dimensional liquid chromatography (LC × LC), solvents of high eluotropic strength are frequently used in the first dimension ( 1 D), which lead to peak broadening in the second dimension ( 2 D). In the majority of the current LC × LC column combinations, analytes are less than optimally refocused upon transfer to the second column, which negatively affects sensitivity. Furthermore, the typical combination of 1 or 2.1 mm columns in the 1 D paired with a 3 mm (or broader) column in the 2 D leads to at least a 9-or 4-fold dilution and a corresponding loss of sensitivity when using concentration-sensitive detectors. This occurs due to the enhanced radial dilution of the analytes in a broader column, while the sensitivity problem is further exacerbated in LC × LC due to the high flow operated 2 D. In this paper, we introduce a solution to neutralize and inverse this dilution problem through a reconcentrating solution using temperature-responsive liquid chromatography (TRLC) in the 1 D, which is a purely aqueous separation mode. Full solute refocusing at the 2 D column head is thereby obtained when TRLC is combined with reversed-phase liquid chromatography (RPLC). This is shown for the combination of a 2.1 mm I.D. TRLC column with decreasing RPLC column diameters (3−2.1−1 mm) operated at the same linear velocities, hence a resulting decrease in dilution, respectively. Ultraviolet (UV) and electrospray ionization time-of-flight mass spectrometry (ESI-TOF-MS) detection were used to determine the experimental detection limits. Sensitivity improvements with UV detection were somewhat lower than expected, but represent ∼1.5and 3-fold sensitivity enhancement when using a 1 mm I.D. column compared to 2.1 or 3 mm I.D. columns in the 2 D, respectively. This is attributed to extra-column dispersion and the poorer performance of 1 mm I.D. columns. A major benefit of the use of 1 mm I.D. columns in the 2 D is that it allows split-free coupling of 2 D effluent with ESI-MS (at 450 μL/min), making the coupling robust and simple. When using ESI-MS even better, albeit more variable, sensitivity enhancements were obtained on the narrower columns. The benefits of the methodology are demonstrated for paraben test solutes and for phenolic compounds in a blueberry extract by TRLC × RPLC-UV-ESI-TOF-MS.

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Section: Resultsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

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Enhanced Sensitivity in Comprehensive Liquid Chromatography: Overcoming the Dilution Problem in LC × LC via Temperature-Responsive Liquid Chromatography

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“…The most commonly used phase systems are RP × RP followed by a combination of RP with hydrophilic interaction liquid chromatography. Although the two-dimensional LC method has not yet been reported for the analysis of polyphenolic compounds in balsamic vinegar samples, it is widely applied for the analysis of polyphenols in grapes and other products of grapes [20,21], for example, wine samples [22,23].…”

Section: Introductionmentioning

confidence: 99%

Comparison of Phenolic Profile of Balsamic Vinegars Determined Using Liquid and Gas Chromatography Coupled with Mass Spectrometry

et al. 2022

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Balsamic vinegar is one of the best known and most popular types of vinegar, and it is a rich source of polyphenolic compounds. The quality of balsamic vinegar as well as the content of phenolic substances vary depending on the production method. In the present work, we have developed a method for comprehensive characterization of the content of phenolic compounds in balsamic vinegars based on the combination of gas chromatography (GC) and high-performance liquid chromatography (HPLC) coupled with mass spectrometric detection in single mode (MS) and tandem mode (MS/MS). In total, 14 samples of different types of balsamic vinegar were analyzed without difficulty in sample preparation. The separation conditions and detection parameters of HPLC-MS/MS were optimized and used for the determination of 29 phenolic compounds and 6 phenolic acids. The profile of phenolic compounds was completed by semi-quantitative analysis of volatile organic compounds using GC-MS after optimized headspace solid-phase microextraction. Gallic acid, protocatechuic acid, caffeic acid, and p-coumaric acid have been identified as the major phenolic compounds in balsamic vinegars.

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“…Phenolic acids in Salvia miltiorrhiza [11], ginsenosides in Panax ginseng [12] and Panax notoginseng [13], sphingolipids in Caenorhabditis elegans [14], and proteins in tissues [15] have been comprehensively characterized using 2D-HILIC × RPLC, which demonstrate its enhanced separation efficiency, reduced ion suppression for the subsequent MS detection, and powerful characterization ability. Other orthogonal separation systems, including 2D-NPLC × RPLC [16], 2D-SEC × RPLC [17][18][19], 2D-chiral × chiral [20], and 2D-achiral × chiral [21], temperatureresponsive LC × RPLC [22], countercurrent chromatography × RPLC [23], IEC × assay-based RPLC [24], SFC × RPLC [25], IPC × RPLC [26], and IEC × SEC [27] have also been developed and applied toward the analysis of biosamples. Moreover, advanced strategies [28][29][30] were proposed for the development of a more systematic, less tedious, and less reliant on user expertise 2D-LC method.…”

Section: Introductionmentioning

confidence: 99%

Comprehensive profiling of Sanguisorba officinalis using offline two‐dimensional mixed‐mode liquid chromatography × reversed‐phase liquid chromatography, tandem high‐resolution mass spectrometry, and molecular network

Dai

Zhang

Xiong

et al. 2022

J of Separation Science

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The profiling of natural products is important in modern biological sciences and new drug development. However, the separation and characterization of complex herbal extracts are significantly challenging for researchers in the biochemical field. Herein, an offline two-dimensional mixed-mode liquid chromatography × reversed-phase liquid chromatography system is developed. Our system exhibits high orthogonality and is composed of a newly prepared stationary phase in the first dimension and a traditional C 18 phase in the second dimension, and is operated in combination with a high-resolution mass spectrometry and molecular network. Sanguisorba officinalis L. is studied using the proposed method owing to its bioactivity. With the aid of orthogonal separation, the ionization of the individual components is improved. The number of detected compounds and separated peaks are significantly increased when one-dimensional liquid chromatography is upgraded to two-dimensional liquid chromatography.In addition, 270 compounds (127 of which are tentatively characterized as new compounds, and further confirmation is needed) are successfully characterized based on their fragmentation patterns under the guidance of molecular network, while only 95 compounds are characterized using one-dimensional liquid chromatography and high-resolution mass spectrometry. The results indicate that the developed offline two-dimensional mixed-mode liquid chromatography ×

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Comprehensive two-dimensional temperature-responsive × reversed phase liquid chromatography for the analysis of wine phenolics

Cited by 21 publications

References 68 publications

Enhanced Sensitivity in Comprehensive Liquid Chromatography: Overcoming the Dilution Problem in LC × LC via Temperature-Responsive Liquid Chromatography

Enhanced Sensitivity in Comprehensive Liquid Chromatography: Overcoming the Dilution Problem in LC × LC via Temperature-Responsive Liquid Chromatography

Comparison of Phenolic Profile of Balsamic Vinegars Determined Using Liquid and Gas Chromatography Coupled with Mass Spectrometry

Comprehensive profiling of Sanguisorba officinalis using offline two‐dimensional mixed‐mode liquid chromatography × reversed‐phase liquid chromatography, tandem high‐resolution mass spectrometry, and molecular network

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