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

doi:10.1002/rcm.4433

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

Research output: Contribution to journal › Article › peer-review

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.

Original language	English
Pages (from-to)	651-658
Journal	Rapid Communications in Mass Spectrometry
Volume	24
Issue number	5
DOIs	https://doi.org/10.1002/rcm.4433
Publication status	Published - Mar 2010

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@article{ec601932778e49178e5e8ff68c23a4f0,

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",

month = mar,

doi = "10.1002/rcm.4433",

language = "English",

volume = "24",

pages = "651--658",

journal = "Rapid Communications in Mass Spectrometry",

issn = "0951-4198",

publisher = "John Wiley & Sons, Inc.",

number = "5",

}

Smyth, TJP, Rodriguez Robledo, V & Smyth, F 2010, 'Characterisation of oxazepam degradation products by high-performance liquid chromatography/electrospray ionisation mass spectrometry and electrospray ionisation quadrupole time-of-flight tandem mass spectrometry', Rapid Communications in Mass Spectrometry, vol. 24, no. 5, pp. 651-658. https://doi.org/10.1002/rcm.4433

Characterisation of oxazepam degradation products by high-performance liquid chromatography/electrospray ionisation mass spectrometry and electrospray ionisation quadrupole time-of-flight tandem mass spectrometry. / Smyth, Thomas J. P.; Rodriguez Robledo, Virginia; Smyth, Franklin.

In: Rapid Communications in Mass Spectrometry, Vol. 24, No. 5, 03.2010, p. 651-658.

Research output: Contribution to journal › Article › peer-review

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.

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DO - 10.1002/rcm.4433

M3 - Article

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JO - Rapid Communications in Mass Spectrometry

JF - Rapid Communications in Mass Spectrometry

SN - 0951-4198

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