Theoretical and practical interest in UHPLC technology for 2D-LC

Sarrut, Morgan; Crétier, G.; Heinisch, Sabine

doi:10.1016/j.trac.2014.08.005

Cited by 38 publications

(16 citation statements)

References 59 publications

(80 reference statements)

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“…It is therefore of prime importance to do everything possible to enhance this ratio. As previously discussed [4], this ratio can be expressed by…”

Section: Theoretical Considerationsmentioning

confidence: 99%

“…Over the last decades, on-line comprehensive two-dimensional liquid chromatography (LCxLC) has grown significantly in many application fields [1][2][3][4]. Liquid chromatography provides a wide variety of separation modes including Reversed Phase Liquid Chromatography (RPLC), Normal Phase Liquid Chromatography (NPLC), Size Exclusion Chromatography (SEC), Ion Exchange Chromatography (IEC) and Hydrophilic Interaction Liquid Chromatography (HILIC).…”

Section: Introductionmentioning

confidence: 99%

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Potential and limitations of on-line comprehensive reversed phase liquid chromatography×supercritical fluid chromatography for the separation of neutral compounds: An approach to separate an aqueous extract of bio-oil

Sarrut

Corgier

Crétier

et al. 2015

Journal of Chromatography A

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On-line comprehensive Reversed Phase Liquid Chromatography×Supercritical Fluid Chromatography (RPLCxSFC) was investigated for the separation of complex samples of neutral compounds. The presented approach aimed at overcoming the constraints involved by such a coupling. The search for suitable conditions (stationary phases, injection solvent, injection volume, design of interface) are discussed with a view of ensuring a good transfer of the compounds between both dimensions, thereby allowing high effective peak capacity in the second dimension. Instrumental aspects that are of prime importance in on-line 2D separations, were also tackled (dwell volume, extra column volume and detection). After extensive preliminary studies, an on-line RPLCxSFC separation of a bio-oil aqueous extract was carried out and compared to an on-line RPLCxRPLC separation of the same sample in terms of orthogonality, peak capacity and sensitivity. Both separations were achieved in 100min. For this sample and in these optimized conditions, it is shown that RPLCxSFC (with Hypercarb and Acquity BEH-2EP as stationary phases in first and second dimension respectively) can generate a slightly higher peak capacity than RPLCxRPLC (with Hypercarb and Acquity CSH phenyl-hexyl as stationary phases in first and second dimension respectively) (620 vs 560). Such a result is essentially due to the high degree of orthogonality between RPLC and SFC which may balance for lesser peak efficiency obtained with SFC as second dimension. Finally, even though current limitations in SFC instrumentation (i.e. large extra-column volume, large dwell volume, no ultra-high pressure) can be critical at the moment for on-line 2D-separations, RPLCxSFC appears to be a promising alternative to RPLCxRPLC for the separation of complex samples of neutral compounds.

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“…It is therefore of prime importance to do everything possible to enhance this ratio. As previously discussed [4], this ratio can be expressed by…”

Section: Theoretical Considerationsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Potential and limitations of on-line comprehensive reversed phase liquid chromatography×supercritical fluid chromatography for the separation of neutral compounds: An approach to separate an aqueous extract of bio-oil

Sarrut

Corgier

Crétier

et al. 2015

Journal of Chromatography A

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“…It is important to notice here that the dilution factor D F is higher for the CPCxLC separation which can lead to some detection problems. As described in the following equation , the dilution factor depends on the peak width observed on first‐dimension and the compression factor. For CPCxLC, despite a high compression factor during transfer, the dramatically low efficiency of the CPC technique leads to a large peak width hence a high dilution factor in the order of 75, in opposition to a dilution factor of 17 in prepLCxLC.…”

Section: Resultsmentioning

confidence: 99%

Comparison between centrifugal partition chromatography and preparative liquid chromatography as first dimensions in off‐line two‐dimensional separation: Application to the isolation of multi‐targeted compounds from Edelweiss plant

2018

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Preparative two-dimensional chromatography is gaining interest in the elucidation of complex samples as it allows the recovery of a large number of molecules without the risks inherent to tedious multi-step sample preparation. While the second dimension is often selected to be liquid chromatography, it may be of interest to compare the specificities of two different techniques, namely liquid chromatography and centrifugal partition chromatography, to be used as first dimension. A fair comparison between off-line CPCxLC and prepLCxLC in selective comprehensive mode for preparative purposes is carried out in this study, illustrated by the isolation of five compounds from high-value Edelweiss plant. The method development of each configuration is achieved on laboratory scale instruments. The quality of separation is compared using 2D-contour plots. The prepLCxLC exhibits a large separation space that leads to an overall large peak capacity, which is of great interest for complex samples. But its limited loading capacity involves a large number of D runs increasing the running costs for preparative purposes. On the other hand, CPCxLC provides a low peak capacity due to the poor efficiency provided by CPC. However, this liquid-liquid technique can be finely tuned to generate a high selectivity, decreasing the number of runs necessary to produce a limited number of target solutes.

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“…The interface cuts the fractions of the primary column effluent and releases them onto the secondary column, where usually a fast separation takes place. The fraction injected onto the secondary column should be completely analyzed before the successive transfer occurs, while the second dimension analysis time should be at least equal or less than the duration of a modulation period . Conventional LC detectors like photo‐diodearray (PDA) and evaporative light scattering (ELSD) can be used in LC × LC, as well as MS and high‐resolution MS (e.g., ToF–MS) by direct on‐line coupling via ionization interfaces such as electrospray ionization (ESI), atmospheric pressure photoionization (APPI), and atmospheric pressure chemical ionization (APCI) .…”

Section: Comprehensive and Hyphenated Chromatographic Techniquesmentioning

confidence: 99%

“…The fraction injected onto the secondary column should be completely analyzed before the successive transfer occurs, while the second dimension analysis time should be at least equal or less than the duration of a modulation period. [98][99][100][101] Conventional LC detectors like photo-diodearray (PDA) and evaporative light scattering (ELSD) can be used in LC × LC, as well as MS and high-resolution MS (e.g., ToF-MS) by direct on-line coupling via ionization interfaces such as electrospray ionization (ESI), atmospheric pressure photoionization (APPI), and atmospheric pressure chemical ionization (APCI). 102 2DLC has many applications in the area of food and pharmaceutical analysis but has also been applied to the analysis of mainly the aqueous phase of bio-oils.…”

Section: Two-dimensional Liquid Chromatography (2dlc or Lc × Lc)mentioning

confidence: 99%

Advanced analytical techniques for bio‐oil characterization

Michailof

Kalogiannis

Sfetsas

et al. 2016

WIREs Energy & Environment

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Bio-oil (pyrolysis oil) is the liquid product of biomass thermochemical conversion. It is a dark, viscous liquid that contains the depolymerization products of hemicellulose, cellulose, and lignin. The physicochemical properties of bio-oils are determined by employing the conventional methods for fuels analysis with proper adaptations. However, the detailed composition of bio-oils in terms of analytes as well as their concentration remains ambiguous and is a challenging task for analytical chemistry. The compounds in the bio-oil range from nonpolar (e.g., hydrocarbons) to highly polar (e.g., phenolics) and from volatile (e.g., organic acids) to nonvolatile (e.g., sugar derivatives), covering a molecular weight (MW) range of about 50-2000 Da. Hence a combination of analytical techniques such as high pressure liquid chromatography, gas chromatography (GC), gel permeation chromatography (GPC), nuclear magnetic resonance spectroscopy (NMR), and Fourier transform infrared spectroscopy (FTIR) are required to determine the bio-oil's composition. Despite the significant breakthroughs of these techniques, they face limitations regarding the sample pretreatment, the incomplete separation and determination of components, and the need of multiple analyses with each method for more complete results. The development of sophisticated, comprehensive, and hyphenated chromatographic and spectrometric techniques such as GC × GC, LC × LC, high-resolution mass spectrometry (HRMS), and 2D-NMR has brought actual advancement in the field of bio-oil analysis. GC × GC and LC × LC have allowed the development of qualitative and quantitative methods for the individual determination of lower MW compounds. However, HRMS and 2D-NMR have facilitated the elucidation of the structure of the higher MW components, offering insight in the effect of pyrolysis conditions on biomass depolymerization and the possibilities for further upgrading of bio-oils.

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Theoretical and practical interest in UHPLC technology for 2D-LC

Cited by 38 publications

References 59 publications

Potential and limitations of on-line comprehensive reversed phase liquid chromatography×supercritical fluid chromatography for the separation of neutral compounds: An approach to separate an aqueous extract of bio-oil

Potential and limitations of on-line comprehensive reversed phase liquid chromatography×supercritical fluid chromatography for the separation of neutral compounds: An approach to separate an aqueous extract of bio-oil

Comparison between centrifugal partition chromatography and preparative liquid chromatography as first dimensions in off‐line two‐dimensional separation: Application to the isolation of multi‐targeted compounds from Edelweiss plant

Advanced analytical techniques for bio‐oil characterization

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