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  1. Article ; Online: Mobile Phase Aging and Its Impact on Electrospray Ionization of Oligonucleotides.

    Guimaraes, Guilherme J / Saad, Jack G / Annavarapu, Vidya / Bartlett, Michael G

    Journal of the American Society for Mass Spectrometry

    2023  Volume 34, Issue 12, Page(s) 2691–2699

    Abstract: The implementation of fluoroalcohol/alkylamine mobile phase systems in oligonucleotide LC-MS provides a good balance between chromatographic separations and MS sensitivity. Since its introduction, several parameters including mobile phase composition, ... ...

    Abstract The implementation of fluoroalcohol/alkylamine mobile phase systems in oligonucleotide LC-MS provides a good balance between chromatographic separations and MS sensitivity. Since its introduction, several parameters including mobile phase composition, additive concentration, alkylamine hydrophobicity, and different fluoroalcohols have been carefully evaluated and optimized. While our understanding of this mobile phase system has increased over the years, there are challenges that continue to hinder method performance and remain poorly understood. One of these challenges is the constant loss of MS sensitivity over time, commonly termed mobile phase aging. This study investigates two aging mechanisms associated with loss of MS sensitivity: alkylamine oxidation and aggregate formation. The relationship between pH, organic solvent, oxygen, and mobile phase aging is characterized, and mitigation strategies to extend mobile phase lifetime are discussed.
    MeSH term(s) Oligonucleotides/chemistry ; Spectrometry, Mass, Electrospray Ionization/methods ; Chromatography, Liquid/methods ; Indicators and Reagents ; Solvents
    Chemical Substances Oligonucleotides ; Indicators and Reagents ; Solvents
    Language English
    Publishing date 2023-11-18
    Publishing country United States
    Document type Journal Article
    ZDB-ID 1073671-2
    ISSN 1879-1123 ; 1044-0305
    ISSN (online) 1879-1123
    ISSN 1044-0305
    DOI 10.1021/jasms.3c00264
    Database MEDical Literature Analysis and Retrieval System OnLINE

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    In stock of ZB MED Cologne/Königswinter

    Zs.A 4618: Show issues Location:
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    bis Jg. 1994: Bestellungen von Artikeln über das Online-Bestellformular
    Jg. 1995 - 2021: Lesesall (2.OG)
    ab Jg. 2022: Lesesaal (EG)
    Zs.MO 241: Show issues

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  2. Article ; Online: Alkylamine ion-pairing reagents and the chromatographic separation of oligonucleotides.

    Li, Ning / El Zahar, N M / Saad, Jack G / van der Hage, Erik R E / Bartlett, Michael G

    Journal of chromatography. A

    2018  Volume 1580, Page(s) 110–119

    Abstract: Alkylamines are commonly used to improve both chromatographic and mass spectral performance of electrospray ionization liquid chromatography mass spectrometry based methods for the analysis of oligonucleotides. Recently several new alkylamines have been ... ...

    Abstract Alkylamines are commonly used to improve both chromatographic and mass spectral performance of electrospray ionization liquid chromatography mass spectrometry based methods for the analysis of oligonucleotides. Recently several new alkylamines have been introduced to enhance the electrospray mass spectral response for oligonucleotides; however, the chromatographic properties of these new alkylamines have not been rigorously assessed. We have investigated the retention, peak width, resolution and general chromatographic performance of fifteen different alkylamines for the separation of a model DNA, RNA and an antisense therapeutic oligonucleotide. Eleven of the fifteen alkylamines were shown to provide similar chromatographic performance across all three classes of oligonucleotides. Based on these findings, a model for the mechanism of retention of oligonucleotides using alkylamines and hexafluoroisopropanol mobile phases is proposed. Depending on the concentrations of alkylamines and pH adjustment, oligonucleotides can be retained by micellar chromatography and not the generally held ion-pairing mechanism. This conclusion is supported by light scattering, transmission electron microscopy and ion mobility experiments detecting three micron aggregates in the mobile phase at concentrations that are routinely used for LC-MS analysis of oligonucleotides. These aggregates are not detected at lower alkylamine concentrations where the retention mechanism follows an ion-pairing mechanism. The formation of these aggregates appears to be dependent on the pH of the mobile phase.
    MeSH term(s) Amines/chemistry ; Chemistry Techniques, Analytical/methods ; Chromatography, Liquid ; DNA/isolation & purification ; Indicators and Reagents/chemistry ; Oligonucleotides/analysis ; Oligonucleotides/isolation & purification ; Propanols/chemistry ; RNA/isolation & purification ; Spectrometry, Mass, Electrospray Ionization ; Tandem Mass Spectrometry
    Chemical Substances Amines ; Indicators and Reagents ; Oligonucleotides ; Propanols ; hexafluoroisopropanol (3D632GYQ50) ; RNA (63231-63-0) ; DNA (9007-49-2)
    Language English
    Publishing date 2018-10-25
    Publishing country Netherlands
    Document type Journal Article
    ZDB-ID 1171488-8
    ISSN 1873-3778 ; 0021-9673
    ISSN (online) 1873-3778
    ISSN 0021-9673
    DOI 10.1016/j.chroma.2018.10.040
    Database MEDical Literature Analysis and Retrieval System OnLINE

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    In stock of ZB MED Cologne/Königswinter

    Zs.A 813: Show issues Location:
    Je nach Verfügbarkeit (siehe Angabe bei Bestand)
    bis Jg. 1994: Bestellungen von Artikeln über das Online-Bestellformular
    Jg. 1995 - 2021: Lesesall (1.OG)
    ab Jg. 2022: Lesesaal (EG)

    Order via subito

    This service is chargeable due to the Delivery terms set by subito. Orders including an article and supplementary material will be classified as separate orders. In these cases, fees will be demanded for each order.

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