Advances in ultra‐high‐pressure and multi‐dimensional liquid chromatography instrumentation and workflows

Vos, Jelle De; Stoll, Dwight R.; Buckenmaier, Stephan; Eeltink, Sebastiaan; Grinias, James P.

doi:10.1002/ansa.202100007

Cited by 19 publications

(7 citation statements)

References 172 publications

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“…Improved HDX MS separations should come from using commercial instrumentation with the highest backpressure limits where higher flow rates are possible. Current [30] major commercial UPLC/UHPLC pump vendors and their system backpressure limits include ThermoScientific (Vanquish) ~21 kpsi; Shimadzu (Nexera) ~19 kpsi; Agilent (Infinity II) ~18 kpsi; Waters (I-Class) ~18 kpsi.…”

Section: Resultsmentioning

confidence: 99%

Increase the flow rate and improve hydrogen deuterium exchange mass spectrometry

Peterle

DePice

Wales

et al. 2022

Preprint

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Reversed-phase peptide separation in hydrogen deuterium exchange (HDX) mass spectrometry (MS) must be done with conditions where the back exchange is the slowest possible, the so-called quench conditions of low pH and low temperature. To retain maximum deuterium, separation must also be done as quickly as possible. The low temperature (0 &degC) of quench conditions complicates the separation and leads primarily to a reduction in separation quality and an increase in chromatographic backpressure. To improve the separation in HDX MS, one could use a longer gradient, smaller particles, a different separation mechanism (for example, capillary electrophoresis), or multi-dimensional separations such as combining ion mobility separation with reversed-phase separation. Another way to improve separations under HDX MS quench conditions is to use a higher flow rate where separation efficiency at 0 &degC is more ideal. Higher flow rates, however, require chromatographic systems (both pumps and fittings) with higher backpressure limits. We tested what improvements could be realized with a commercial UHPLC/UPLC system capable of ~20,000 psi backpressure. We found that a maximum flow rate of 225 uL/min was possible and that higher flow rate clearly led to higher peak capacity. HDX MS analysis of both simple and particularly complex samples improved, permitting both shorter separation time, if desired, and providing more deuterium recovery.

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Section: Resultsmentioning

confidence: 99%

Increase the flow rate and improve hydrogen deuterium exchange mass spectrometry

Peterle

DePice

Wales

et al. 2022

Preprint

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“…Recently, 2D‐LC 41 has been applied to oligonucleotides. Li and Lämmerhofer developed a method to evaluate the impurities present from the antisense strand of Patisiran by using three different 2D‐LC platforms 42 .…”

Section: Advances In the Characterisation Of Oligonucleotides By 2d‐lcmentioning

confidence: 99%

Advancements in the characterisation of oligonucleotides by high performance liquid chromatography‐mass spectrometry in 2021: A short review

Black

Ray

Stulz

et al. 2022

Analytical Science Advances

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The first oligonucleotide therapeutic was approved by the Food and Drug Administration in 1998, and since then, 12 nucleic acids have been commercialised as medicines. To be approved, the oligonucleotides need to be identified and characterised as well as its related impurities. Different methods exist, but the most commonly used is ion‐pairing reversed‐phase liquid chromatography with tandem mass spectrometry. The separation obtained depends on the mobile phase and column used. Other methods have been developed, notably by using hydrophilic interaction chromatography and two‐dimensional high performance liquid chromatography. Furthermore, ion‐pairing reversed‐phase high performance liquid chromatography ultra‐violet spectroscopy detection and mass spectrometry has been optimised for the analysis of methylated nucleobases due to the utilisation of this modification in the drugs. This review covers the recent advancements in the analysis and characterisation of oligonucleotides in 2021 by high performance liquid chromatography mass spectrometry, notably by hydrophilic interaction chromatography and two‐dimensional liquid chromatography but also the different parameters that influence the analysis by ion‐pairing reversed‐phase high performance liquid chromatography, the characterisation of methylated nucleobases, and the recent software developed for oligonucleotides.

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“…Furthermore, it shows that over the course of several decades the core of the technology has apparently not changed a lot (i.e., the columns still look exactly the same) but the technique is so powerful that it definitely deserves to be highlighted. The last atom shows a peak pattern that needs to be resolved based on the paper by De Vos et al 11 . The three different "overlapping" chromatograms show how information from multiple dimensions of separation are required to provide the required information.…”

Section: Figurementioning

confidence: 99%

Annual Reviews 2020: Recent advances in analytical sciences

Eeltink

2021

Analytical Science Advances

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This issue of Analytical Science Advances includes review papers written by authorities in the field, covering a wide range of topics in the field of analytical sciences. Authors were asked to provide a critical review discussing the state-of-the-art in their field and highlight the key developments and applications covering the literature published in 2020. These reviews are ideally suited for those who want a rapid overview of the latest advances in a particular field and learn about emerging applications. Mass spectrometry (MS) is an immensely important analytical technology that still rapidly develops and continues to find new application areas. In their review on the rise of single-cell proteomics, Ctortecka and Mechtler discuss the current state-of-the-art MS-based workflows. In particular, aspects of sample preparation when working with minute amounts of samples are discussed, new possibilities in separation science are highlighted, and emerging MS quantification strategies including data postprocessing are discussed. An overview of the current capabilities of high-resolution MS and its applicability to pharmaceutical analysis is provided by Géhin and Holman. Rankin-Turner and Heaney discuss new technological advances in ambient ionization MS and provide an overview of key paper published in biomedical sciences, forensics and security, food sciences, the environment, and chemical synthesis. The Hoffmann group summarizes the latest developments in MS imaging, with a focus on the latest approaches for tissue-based imaging. Several topics are covered in the field of separation science. De Vos et al. summarize the latest advances in UHPLC and multi-dimensional LC instrument development and highlight recent key applications. The Franchina group reports on the latest instrumental advances and applications of comprehensive two-dimensional gas chromatography (GC × GC), including its hyphenation with novel upstream or downstream processes. Major applied fields such as energy, fuel, foodstuff, plant, biological, and environmental are also covered. The analysis of low molecular weight polar and ionic components using ion chromatography (IC) coupled to MS is summarized by Bruggink and Jensen. Further applications using IC hyphenated to inductively coupled plasma mass spectrometric detection are reviewed. Muza et al. described the recent advances in designing and fabricating bioconjugated and selfassembled polymer structures and their characterization using field flow fractionation. The latter separation technique utilizes fluid flow dynamics and external force fields for effective separations at steadystate conditions within a solvent filled channel. Finally, Eeltink et al.

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Advances in ultra‐high‐pressure and multi‐dimensional liquid chromatography instrumentation and workflows

Cited by 19 publications

References 172 publications

Increase the flow rate and improve hydrogen deuterium exchange mass spectrometry

Increase the flow rate and improve hydrogen deuterium exchange mass spectrometry

Advancements in the characterisation of oligonucleotides by high performance liquid chromatography‐mass spectrometry in 2021: A short review

Annual Reviews 2020: Recent advances in analytical sciences

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