Stable-bond polymeric reversed-phase/weak anion-exchange mixed-mode stationary phases obtained by simultaneous functionalization and crosslinking of a poly(3-mercaptopropyl)methylsiloxane-film on vinyl silica via thiol-ene double click reaction

Bäurer, Stefanie; Zimmermann, Aleksandra; Woiwode, Ulrich; Sánchez-Muñoz, Orlando L.; Krämer, M.; Horak, Jeannie; Lindner, Wolfgang; Bicker, Wolfgang; Lämmerhofer, Michael

doi:10.1016/j.chroma.2019.01.078

Cited by 22 publications

(10 citation statements)

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“…1–14), but suffer from low efficiencies 9 . In recent work to improve the hydrolytic stability of silica‐based mixed‐mode RP/AX materials, a polymer‐coating approach was used 10 . The resulting stationary phase was shown to have good stability when used with a pH 5 mobile phase at 60°C.…”

Section: Introductionmentioning

confidence: 99%

Electrospray ionization mass spectrometry ion suppression/enhancement caused by column bleed for three mixed‐mode reversed‐phase/anion‐exchange high‐performance liquid chromatography columns

Walter

Boissel

2021

Rapid Comm Mass Spectrometry

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Rationale Mixed‐mode reversed‐phase/anion exchange liquid chromatography is useful for separations of mixtures containing anions (e.g. ionized acids). However, when using this form of liquid chromatography with mass spectrometry detection, the bleed of amine‐containing hydrolysis products from the columns may cause ion suppression or enhancement. Methods Using electrospray ionization tandem quadrupole mass spectrometry detection, we determined the ion suppression or enhancement caused by column bleed for three mixed‐mode reversed‐phase/weak anion‐exchange columns containing stationary phases that differ in chemical structure. Two of the stationary phases are based on silica particles, while the third uses ethylene‐bridged hybrid organic/inorganic particles, which have improved hydrolytic stability. Mixtures of acidic and basic analytes were combined with the chromatography flow postcolumn, both with and without a column, and their mass spectrometry ion signal responses (peak areas) were determined. The ratio of signal response with and without a column is the matrix factor. Positive ion electrospray measurements were carried out using 0.1% formic acid (pH ~ 2.7) as a mobile phase additive, and 10mM ammonium formate (pH ~ 6.4) was used for negative ion electrospray detection. Results The matrix factors under both positive and negative ionization modes were closest to 1 (0.74–1.16) for the hybrid particle‐based columns, showing minimal ion suppression or enhancement. In contrast, the silica‐based columns gave matrix factors ranging from 0.04 to 1.86, indicating high levels of ion suppression or enhancement. These results may be explained by the differences in the structures of the stationary phases, which affect the relative amounts of hydrolysis products that elute from the columns. Conclusions The low levels of mass spectrometry ion suppression or enhancement caused by column bleed from the hybrid particle‐based columns should allow for accurate quantitative mass spectrometric detection combined with mixed‐mode reversed‐phase/weak anion‐exchange chromatography.

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Section: Introductionmentioning

confidence: 99%

Electrospray ionization mass spectrometry ion suppression/enhancement caused by column bleed for three mixed‐mode reversed‐phase/anion‐exchange high‐performance liquid chromatography columns

Walter

Boissel

2021

Rapid Comm Mass Spectrometry

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“…These bonded phases may also exhibit instability with basic mobile phases, due to dissolution of the silica particles [16]. Elution of bonded phase hydrolysis products containing amine groups from these stationary phases may interfere with ESI MS detection [17,18]. Organic polymer-based mixed-mode columns have been reported to be stable over a wide pH range (e.g., [1][2][3][4][5][6][7][8][9][10][11][12][13][14], but suffer from low efficiencies [19].…”

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confidence: 99%

“…Organic polymer-based mixed-mode columns have been reported to be stable over a wide pH range (e.g., [1][2][3][4][5][6][7][8][9][10][11][12][13][14], but suffer from low efficiencies [19]. Recent work to improve the hydrolytic stability of silica-based mixedmode RP/AX materials used a polymer-coating approach and functionalization via thiol-ene click reactions [18]. The resulting stationary phase was shown to have good stability when used with a pH 5 mobile phase at 60 • C.…”

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“…The results are compared to those obtained for three RP stationary phases: BEH C 18 , high strength silica (HSS) T3, and charged surface hybrid (CSH) C 18 . These materials were chosen as benchmarks because they are widely used and share several characteristics with BEH C 18 AX columns: the BEH particle chemistry (for BEH C 18 and CSH C 18 ) [20], the intermediate coverage C 18 bonded phase (for HSS T3) [21], and the presence of both C 18 and AX groups (for CSH C 18 ) [22,23].…”

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confidence: 99%

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Characterization of a highly stable mixed‐mode reversed‐phase/weak anion‐exchange stationary phase based on hybrid organic/inorganic particles

Walter

Alden

Field

et al. 2021

J of Separation Science

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We have characterized Atlantis ethylene‐bridged hybrid C18 anion‐exchange, a mixed‐mode reversed‐phase/weak anion‐exchange stationary phase designed to give greater retention for anions (e.g., ionized acids) compared to conventional reversed‐phase materials. The retention and selectivity of this stationary phase were compared to that of three benchmark materials, using a mixture of six polar compounds that includes an acid, two bases, and three neutrals. The compatibility of the ethylene‐bridged hybrid C18 anion‐exchange material with 100% aqueous mobile phases was also evaluated. We investigated the batch‐to‐batch reproducibility of the ethylene‐bridged hybrid C18 anion‐exchange stationary phase for 27 batches across three different particle sizes (1.7, 2.5, and 5 μm) and found it to be comparable to that of one of the most reproducible C18 stationary phases. We also characterized the acid and base stability of the ethylene‐bridged hybrid C18 anion‐exchange stationary phase and the results show it to be usable over a wide pH range, from 2 to 10. The extended upper pH limit relative to silica‐based reversed‐phase/weak anion‐exchange materials is enabled by the use of ethylene‐bridged hybrid organic/inorganic particles. The improved base stability allows Atlantis ethylene‐bridged hybrid C18 anion‐exchange to be used with a wider range of mobile phase pH values, opening up a greater range of selectivity options.

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“…In a second version, the residual thiols on the polymeric RP/WAX were oxidized to sulfonic acids to obtain a RP/WAX/strong cation exchanger (RP/WAX/SCX) stationary phase. These groups act as surface anchored counterions, shifting the still net positive surface charge to lower ]%' , This modification allowed to accelerate the separation of negatively charged ONs, with a reduction of the total analysis time by about 50%[111].…”

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confidence: 99%

Oligonucleotides: Current Trends and Innovative Applications in the Synthesis, Characterization, and Purification

Catani

Luca

Alcântara

et al. 2020

Biotechnology Journal

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Oligonucleotides (ONs) are gaining increasing importance as a promising novel class of biopharmaceuticals. Thanks to their fundamental role in gene regulation, they can be used to develop custom-made drugs (also called N-to-1) able to act on the gene expression at pretranslational level. With recent approvals of ON-based therapeutics by FDA, a growing demand for high-quality chemically-modified ONs is emerging and their market is expected to impressively prosper in the very next future. To satisfy this growing market demand, a scalable and economically sustainable ON production is needed. In this paper, the state of the art of the whole ON production process is illustrated with the aim of highlighting the most promising routes towards the auspicated market-size production. In particular, the most recent advancements in both the upstream stage, mainly based on solid-phase synthesis and recombinant technology, and the downstream one, focusing on chromatographic techniques, are reviewed. Since ON production is projected to expand to the large scale, automatized multi-column technologies will reasonably be required soon to replace the current ones based on batch single-column operations. Cutting edge purification solutions, based on continuous chromatography, will be thus presented in the last part of this review.

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Stable-bond polymeric reversed-phase/weak anion-exchange mixed-mode stationary phases obtained by simultaneous functionalization and crosslinking of a poly(3-mercaptopropyl)methylsiloxane-film on vinyl silica via thiol-ene double click reaction

Cited by 22 publications

References 50 publications

Electrospray ionization mass spectrometry ion suppression/enhancement caused by column bleed for three mixed‐mode reversed‐phase/anion‐exchange high‐performance liquid chromatography columns

Electrospray ionization mass spectrometry ion suppression/enhancement caused by column bleed for three mixed‐mode reversed‐phase/anion‐exchange high‐performance liquid chromatography columns

Characterization of a highly stable mixed‐mode reversed‐phase/weak anion‐exchange stationary phase based on hybrid organic/inorganic particles

Oligonucleotides: Current Trends and Innovative Applications in the Synthesis, Characterization, and Purification

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