History, Evolution, and Optimization Aspects of Comprehensive Two‐Dimensional Liquid Chromatography

François, Isabelle; Sandra, Koen; Sandra, Pat

doi:10.1002/9781118003466.ch8

Cited by 4 publications

(4 citation statements)

References 146 publications

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“…As is often found in the literature, ,,− the online LC × LC interface consists of a two-loop modulation composed of a single two-position 10-port valve. In contrast to many interfaces of this type, counter-flow emptying of one of the two loops is used for the benefit of equal capillary volumes in D2 comparing both valve positions.…”

Section: Methodsmentioning

confidence: 99%

“…Upper tolerable flow rate limits of common electrospray ionization (ESI) sources are approximately 1 mL min –1 , and for atmospheric pressure chemical ionization (APCI), they are 2 mL min –1 ; however, these values are already far above the optimum. The necessity for a flow split inevitably adds losses of sensitivity …”

mentioning

confidence: 99%

“…Besides the possible interface overload, the practitioner has to pay attention to the data acquisition rate of the respective mass spectrometer, especially if older quadrupole-based MS systems are used, as resulting peak widths for short D2 runs can be 1–2 s and below . Although fast-scanning systems of the latest generation may be capable of measuring the minimum-needed 6 to 10 data points per peak under certain conditions (e.g., reduced mass-to-charge ratio ( m / z ) range), it is recommended in the literature to switch to time-of-flight (TOF) type MS as the high data acquisition rates are more than sufficient and independent of the selected m / z range. , The application of multiple D2 systems operated in parallel allows decreasing the critical D2 speed; − however, besides increased complexity, additional hardware such as columns, valves, and costly MS detectors would be necessary. The alternate use of stop-flow methods also allows for a sufficient number of D1 eluate samples, but overall analysis time is drastically increased because the D1 has to be stopped after each eluate sample to allow the D2 separation to be performed. − …”

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confidence: 99%

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Online and Splitless NanoLC × CapillaryLC with Quadrupole/Time-of-Flight Mass Spectrometric Detection for Comprehensive Screening Analysis of Complex Samples

et al. 2013

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A novel multidimensional separation system based on online comprehensive two-dimensional liquid chromatography and hybrid high-resolution mass spectrometry has been developed for the qualitative screening analysis and characterization of complex samples. The core of the system is a consistently miniaturized two-dimensional liquid chromatography that makes the rapid second dimension compatible with mass spectrometry without the need for any flow split. Elevated temperature, ultrahigh pressure, and a superficially porous sub-3-μm stationary phase provide a fast second dimension separation and a sufficient sampling frequency without a first dimension flow stop. A highly loadable porous graphitic carbon stationary phase is employed in the first dimension to implement large volume injections that help countervailing dilution caused by the sampling process between the two dimensions. Exemplarily, separations of a 99-component standard mixture and a complex wastewater sample were used to demonstrate the performance of the dual-gradient system. In the second dimension, 30 s gradients at a cycle time of 1 min were employed. One multidimensional separation took 80-90 min (~120 min including extended hold and re-equilibration in the first dimension). This approach represents a cost-efficient alternative to online LC × LC strategies working with conventionally sized columns in the rapid second dimension, as solvent consumption is drastically decreased and analytes still are detectable at environmentally relevant concentrations.

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Section: Methodsmentioning

confidence: 99%

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confidence: 99%

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confidence: 99%

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Online and Splitless NanoLC × CapillaryLC with Quadrupole/Time-of-Flight Mass Spectrometric Detection for Comprehensive Screening Analysis of Complex Samples

et al. 2013

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“…The valve shown here has a symmetrical 8-port, 2-position design. Many other valve configurations have been described in the literature; the most comprehensive discussion of these options have been given by Schure and Cohen and Francois, Sandra, and Sandra …”

Section: Different Implementations Of 2d-lc Can Be Used To Address Di...mentioning

confidence: 99%

Two-Dimensional Liquid Chromatography: A State of the Art Tutorial

2016

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In this tutorial, we discuss the motivations for doing two-dimensional liquid chromatography (2D-LC) and describe the commonly used implementations of the method. We review important guiding principles for method development, discuss the state of the art in 2D-LC performance as measured by peak capacity, and describe example applications from different fields that we hope will inspire new users to adopt 2D-LC for their analytical problems.

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Comprehensive two-dimensional liquid chromatography of therapeutic monoclonal antibody digests

et al. 2014

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Comprehensive two-dimensional liquid chromatography (LC×LC) is here proposed as a novel tool for peptide mapping of therapeutic monoclonal antibodies in both R&D and routine (QA/QC) environments. This is illustrated by the analysis of the tryptic digest of trastuzumab (Herceptin) applying a commercially available two-dimensional 2D-LC system. Three different LC×LC combinations, i.e., strong cation-exchange × reversed-phase (SCX×RP), reversed-phase × reversed-phase (RP×RP), and hydrophilic interaction × reversed-phase (HILIC×RP), are reported. Detection was carried out using both UV detection (DAD) and mass spectrometry (MS). Several challenges related to the application of LC×LC in peptide mapping and the hyphenation to MS are addressed. The applicability of LC×LC in the assessment of identity, purity, and comparability is demonstrated by the analysis of different Herceptin innovator production batches, a Herceptin biosimilar in development and of stressed samples. The described methodology was shown to be precise in terms of peak volume and (2)D retention time opening interesting perspectives for use in QA/QC testing.

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History, Evolution, and Optimization Aspects of Comprehensive Two‐Dimensional Liquid Chromatography

Cited by 4 publications

References 146 publications

Online and Splitless NanoLC × CapillaryLC with Quadrupole/Time-of-Flight Mass Spectrometric Detection for Comprehensive Screening Analysis of Complex Samples

Online and Splitless NanoLC × CapillaryLC with Quadrupole/Time-of-Flight Mass Spectrometric Detection for Comprehensive Screening Analysis of Complex Samples

Two-Dimensional Liquid Chromatography: A State of the Art Tutorial

Comprehensive two-dimensional liquid chromatography of therapeutic monoclonal antibody digests

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