Using pure shift HSQC to characterize microgram samples of drug metabolites

Liu, Yong; Green, Mitchell D.; Marques, Rosemary; Pereira, Tony; Helmy, Roy; Williamson, R. Thomas; Bermel, Wolfgang; Martin, Gary E.

doi:10.1016/j.tetlet.2014.06.067

Cited by 22 publications

(25 citation statements)

References 11 publications

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“…Standard 1 H and 13 C reference spectra were acquired followed by a multiplicity‐edited pure shift HSQC spectrum . An Inverted Direct Response (IDR) HSQC‐TOCSY spectrum with an 18 ms mixing time was used to establish the homonuclear proton‐proton connectivity network and to sort it by 13 C chemical shifts .…”

Section: Methodsmentioning

confidence: 99%

“…Standard 1 H and 13 C reference spectra were acquired followed by a multiplicity-edited pure shift HSQC spectrum. [8,9] An Inverted Direct Response (IDR) HSQC-TOCSY spectrum with an 18 ms mixing time was used to establish the homonuclear proton-proton connectivity network and to sort it by 13 C chemical shifts. [10] Long-range heteronuclear 1 H-13 C and 1 H-15 N correlations were either established using the HMBC experiment [11] or the more recently developed LR-HSQMBC experiment.…”

Section: Nmrmentioning

confidence: 99%

See 1 more Smart Citation

Unusual (+/–)‐electrospray ionization induced fragmentation: Structural elucidation of an in‐process synthetic intermediate of doravirine (MK‐1439) using liquid chromatography/high‐resolution tandem mass spectrometry and two‐dimensional nuclear magnetic resonance

Sheng

Lexa

Zhang

et al. 2017

Rapid Comm Mass Spectrometry

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Section: Methodsmentioning

confidence: 99%

Section: Nmrmentioning

confidence: 99%

Unusual (+/–)‐electrospray ionization induced fragmentation: Structural elucidation of an in‐process synthetic intermediate of doravirine (MK‐1439) using liquid chromatography/high‐resolution tandem mass spectrometry and two‐dimensional nuclear magnetic resonance

Sheng

Lexa

Zhang

et al. 2017

Rapid Comm Mass Spectrometry

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“…The BIRD‐based homodecoupling method has been further refined and adapted for pure shift 1D and 2D HSQC experiments and applied in a variety of structural problems …”

Section: Broadband Homodecoupling Building Blocksmentioning

confidence: 99%

Broadband¹H homodecoupled NMR experiments: recent developments, methods and applications

2015

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In recent years, a great interest in the development of new broadband 1H homonuclear decoupled techniques providing simplified JHH multiplet patterns has emerged again in the field of small molecule NMR. The resulting highly resolved 1H NMR spectra display resonances as collapsed singlets, therefore minimizing signal overlap and expediting spectral analysis. This review aims at presenting the most recent advances in pure shift NMR spectroscopy, with a particular emphasis to the Zangger-Sterk experiment. A detailed discussion about the most relevant practical aspects in terms of pulse sequence design, selectivity, sensitivity, spectral resolution and performance is provided. Finally, the implementation of the different reported strategies into traditional 1D and 2D NMR experiments is described while several practical applications are also reviewed.

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“…Moreover, important NMR features, such as the development of pulsed Fourier transform NMR spectrometers with high magnetic fields, [44,45] and the development of powerful multidimensional experiments has helped in the characterization of complex matrices. [45,46] Additionally, because of the rapid, non-destructive and quantitative nature of NMR experiments, the quantification of specific regions of the spectrum is possible. [47,48] Thus, the following section will discuss important aspects of NMR applied to input and output sewage treatment plants, such as sample preparation, preservation, characterization and quantification.…”

Section: Nmr Applied To the Study Of Wastewatermentioning

confidence: 99%

Advancements in waste water characterization through NMR spectroscopy: review

Filho

Silva

Ferreira

2014

Magnetic Reson in Chemistry

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There are numerous organic pollutants that lead to several types of ecosystem damage and threaten human health. Wastewater treatment plants are responsible for the removal of natural and anthropogenic pollutants from the sewage, and because of this function, they play an important role in the protection of human health and the environment. Nuclear magnetic resonance (NMR) has proven to be a valuable analytical tool as a result of its versatility in characterizing both overall chemical composition as well as individual species in a wide range of mixtures. In addition, NMR can provide physical information (rigidity, dynamics, etc.) as well as permit in depth quantification. Hyphenation with other techniques such as liquid chromatography, solid phase extraction and mass spectrometry creates unprecedented capabilities for the identification of novel and unknown chemical species. Thus, NMR is widely used in the study of different components of wastewater, such as complex organic matter (fulvic and humic acids), sludge and wastewater. This review article summarizes the NMR spectroscopy methods applied in studies of organic pollutants from wastewater to provide an exhaustive review of the literature as well as a guide for readers interested in this topic.

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Using pure shift HSQC to characterize microgram samples of drug metabolites

Cited by 22 publications

References 11 publications

Unusual (+/–)‐electrospray ionization induced fragmentation: Structural elucidation of an in‐process synthetic intermediate of doravirine (MK‐1439) using liquid chromatography/high‐resolution tandem mass spectrometry and two‐dimensional nuclear magnetic resonance

Unusual (+/–)‐electrospray ionization induced fragmentation: Structural elucidation of an in‐process synthetic intermediate of doravirine (MK‐1439) using liquid chromatography/high‐resolution tandem mass spectrometry and two‐dimensional nuclear magnetic resonance

Broadband¹H homodecoupled NMR experiments: recent developments, methods and applications

Advancements in waste water characterization through NMR spectroscopy: review

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Using pure shift HSQC to characterize microgram samples of drug metabolites

Cited by 22 publications

References 11 publications

Unusual (+/–)‐electrospray ionization induced fragmentation: Structural elucidation of an in‐process synthetic intermediate of doravirine (MK‐1439) using liquid chromatography/high‐resolution tandem mass spectrometry and two‐dimensional nuclear magnetic resonance

Unusual (+/–)‐electrospray ionization induced fragmentation: Structural elucidation of an in‐process synthetic intermediate of doravirine (MK‐1439) using liquid chromatography/high‐resolution tandem mass spectrometry and two‐dimensional nuclear magnetic resonance

Broadband1H homodecoupled NMR experiments: recent developments, methods and applications

Advancements in waste water characterization through NMR spectroscopy: review

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Broadband¹H homodecoupled NMR experiments: recent developments, methods and applications