Temperature dependent 15N NMR study of nitric oxide

Khan, Arafat Hossain; Michel, D.; Bertmer, Marko

doi:10.1016/j.ssnmr.2019.05.002

Cited by 3 publications

(1 citation statement)

References 36 publications

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“…The main aim of the present study was to establish the nature of degradation impurities that involved enrichment, isolation, and characterization of degradation impurities, and the development and validation of suitable stability-indicating analytical method. Liquid chromatography-mass spectrometry (LC-MS), high-resolution mass spectrometry (HR-MS) [9][10][11][12][13][14], and two-dimensional nuclear magnetic resonance (2D NMR) spectroscopy [15][16][17][18][19][20][21][22] techniques have been extensively used as powerful technologies in identifying and characterizing DPs.…”

Section: Introductionmentioning

confidence: 99%

Stress degradation study of Etoricoxib, isolation, and characterization of major degradation impurity by preparative high‐performance liquid chromatography, liquid chromatography‐mass spectrometry, and nuclear magnetic resonance: Validation of ultra‐performance liquid chromatography method

Goguladinne,

Shyamala,

Rao

2024

Separation Science Plus

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Etoricoxib (ETO) is a selective cyclooxygenase‐2 inhibitor, used as a nonsteroidal anti‐inflammatory drug. In this study, a detailed investigation was conducted on the degradation behavior of ETO under acidic, basic, neutral, photolytic, oxidative, and thermal degradation conditions as per the International Conference on Harmonization (ICH) guideline Q1A (R2). A gradient “ultra‐performance liquid chromatography (UPLC)” method was developed for separating the degradation products formed under various degradation conditions along with process‐related impurities. Acquity BEH phenyl column was used for the separation of analytes and 0.1% formic acid in water and 0.05% formic acid in acetonitrile:methanol (8:2 %v/v) were used as mobile phase‐A and mobile phase‐B. A major degradant namely, N‐oxide impurity was observed in oxidative degradation along with two minor degradants where N‐oxide was confirmed based on LC‐mass spectrometry (LC‐MS) studies. Further, the major degradant was enriched and isolated using preparative HPLC and the conformation of the N‐oxide impurity was established using nuclear magnetic resonance techniques including two‐dimensional studies and high‐resolution MS. In addition, the method for related substances by UPLC has been validated by considering a major degradant, namely N‐oxide along with process‐related impurities as per the ICH guidelines validation parameters.

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Section: Introductionmentioning

confidence: 99%

Stress degradation study of Etoricoxib, isolation, and characterization of major degradation impurity by preparative high‐performance liquid chromatography, liquid chromatography‐mass spectrometry, and nuclear magnetic resonance: Validation of ultra‐performance liquid chromatography method

Goguladinne,

Shyamala,

Rao

2024

Separation Science Plus

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Solid-state NMR of small molecule adsorption in metal–organic frameworks (MOFs)

Bertmer

2020

Annual Reports on NMR Spectroscopy

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Nuclear spin relaxation

Kowalewski¹

2020

Nuclear Magnetic Resonance

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The review covers the progress in the field of NMR relaxation in fluids primarily during 2019. Since the topic is returning to this volume SPR after a break of a few years, some highlights of the relaxation literature from the period 2014–18 are mentioned. The emphasis is on comparatively simple liquids and solutions of physico-chemical and chemical interest, as in previous periods, but selected biophysics-related topics (including some work on relaxation in solid biomaterials) and relaxation-related studies on more complex systems (macromolecular solutions, liquid crystalline systems, glassy and porous materials) are also covered. Section 2 of the chapter is concerned with general, physical and experimental aspects of nuclear spin relaxation, while Section 3 is concentrated on applications.

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Temperature dependent 15N NMR study of nitric oxide

Cited by 3 publications

References 36 publications

Stress degradation study of Etoricoxib, isolation, and characterization of major degradation impurity by preparative high‐performance liquid chromatography, liquid chromatography‐mass spectrometry, and nuclear magnetic resonance: Validation of ultra‐performance liquid chromatography method

Stress degradation study of Etoricoxib, isolation, and characterization of major degradation impurity by preparative high‐performance liquid chromatography, liquid chromatography‐mass spectrometry, and nuclear magnetic resonance: Validation of ultra‐performance liquid chromatography method

Solid-state NMR of small molecule adsorption in metal–organic frameworks (MOFs)

Nuclear spin relaxation

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