Characterisation of oxazepam degradation products by high-performance liquid chromatography/electrospray ionisation mass spectrometry and electrospray ionisation quadrupole time-of-flight tandem mass spectrometry

Thomas J. P. Smyth, Virginia Rodriguez Robledo, Franklin Smyth

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    8 Citations (Scopus)

    Abstract

    Oxazepam has been subjected to controlled degradation at 100 degrees C for 3h in 0.5M HCl and 0.5M NaOH. Following neutralisation of the degradation mixture and removal of salts by solid-phase extraction (SPE), isocratic high-performance liquid chromatography/mass spectrometry (HPLC/MS) using water/methanol (25:75 v/v) as the mobile phase was carried out using a flow diverter to collect fractions prior to their characterisation by electrospray ionisation multi-stage mass spectrometry (ESI-MSn) and proposal of the corresponding fragmentation patterns. The elemental compositions of the degradation products and their MS fragments were evaluated using electrospray ionisation quadrupole time-of-flight tandem mass spectrometry (ESI-QTOF-MS/MS) which was then used to support the proposed fragmentation patterns. Copyright (C) 2010 John Wiley & Sons, Ltd.
    LanguageEnglish
    Pages651-658
    JournalRapid Communications in Mass Spectrometry
    Volume24
    Issue number5
    DOIs
    Publication statusPublished - Mar 2010

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    Oxazepam
    Electrospray ionization
    High performance liquid chromatography
    Mass spectrometry
    Degradation
    Methanol
    Salts
    Water
    Chemical analysis

    Cite this

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    title = "Characterisation of oxazepam degradation products by high-performance liquid chromatography/electrospray ionisation mass spectrometry and electrospray ionisation quadrupole time-of-flight tandem mass spectrometry",
    abstract = "Oxazepam has been subjected to controlled degradation at 100 degrees C for 3h in 0.5M HCl and 0.5M NaOH. Following neutralisation of the degradation mixture and removal of salts by solid-phase extraction (SPE), isocratic high-performance liquid chromatography/mass spectrometry (HPLC/MS) using water/methanol (25:75 v/v) as the mobile phase was carried out using a flow diverter to collect fractions prior to their characterisation by electrospray ionisation multi-stage mass spectrometry (ESI-MSn) and proposal of the corresponding fragmentation patterns. The elemental compositions of the degradation products and their MS fragments were evaluated using electrospray ionisation quadrupole time-of-flight tandem mass spectrometry (ESI-QTOF-MS/MS) which was then used to support the proposed fragmentation patterns. Copyright (C) 2010 John Wiley & Sons, Ltd.",
    author = "Smyth, {Thomas J. P.} and {Rodriguez Robledo}, Virginia and Franklin Smyth",
    year = "2010",
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    doi = "10.1002/rcm.4433",
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    journal = "Rapid Communications in Mass Spectrometry",
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    TY - JOUR

    T1 - Characterisation of oxazepam degradation products by high-performance liquid chromatography/electrospray ionisation mass spectrometry and electrospray ionisation quadrupole time-of-flight tandem mass spectrometry

    AU - Smyth, Thomas J. P.

    AU - Rodriguez Robledo, Virginia

    AU - Smyth, Franklin

    PY - 2010/3

    Y1 - 2010/3

    N2 - Oxazepam has been subjected to controlled degradation at 100 degrees C for 3h in 0.5M HCl and 0.5M NaOH. Following neutralisation of the degradation mixture and removal of salts by solid-phase extraction (SPE), isocratic high-performance liquid chromatography/mass spectrometry (HPLC/MS) using water/methanol (25:75 v/v) as the mobile phase was carried out using a flow diverter to collect fractions prior to their characterisation by electrospray ionisation multi-stage mass spectrometry (ESI-MSn) and proposal of the corresponding fragmentation patterns. The elemental compositions of the degradation products and their MS fragments were evaluated using electrospray ionisation quadrupole time-of-flight tandem mass spectrometry (ESI-QTOF-MS/MS) which was then used to support the proposed fragmentation patterns. Copyright (C) 2010 John Wiley & Sons, Ltd.

    AB - Oxazepam has been subjected to controlled degradation at 100 degrees C for 3h in 0.5M HCl and 0.5M NaOH. Following neutralisation of the degradation mixture and removal of salts by solid-phase extraction (SPE), isocratic high-performance liquid chromatography/mass spectrometry (HPLC/MS) using water/methanol (25:75 v/v) as the mobile phase was carried out using a flow diverter to collect fractions prior to their characterisation by electrospray ionisation multi-stage mass spectrometry (ESI-MSn) and proposal of the corresponding fragmentation patterns. The elemental compositions of the degradation products and their MS fragments were evaluated using electrospray ionisation quadrupole time-of-flight tandem mass spectrometry (ESI-QTOF-MS/MS) which was then used to support the proposed fragmentation patterns. Copyright (C) 2010 John Wiley & Sons, Ltd.

    U2 - 10.1002/rcm.4433

    DO - 10.1002/rcm.4433

    M3 - Article

    VL - 24

    SP - 651

    EP - 658

    JO - Rapid Communications in Mass Spectrometry

    T2 - Rapid Communications in Mass Spectrometry

    JF - Rapid Communications in Mass Spectrometry

    SN - 0951-4198

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    ER -