• Title/Summary/Keyword: Solution NMR Sensitivity

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Sensitivity Enhancement in Solution NMR via Photochemically Induced Dynamic Nuclear Polarization

  • Im, Jonghyuk;Lee, Jung Ho
    • Journal of the Korean Magnetic Resonance Society
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    • v.21 no.1
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    • pp.1-6
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    • 2017
  • Enhancements in NMR sensitivity have been the main driving force to extend the boundaries of NMR applications. Recently, techniques to shift the thermally populated nuclear spin states are employed to gain high NMR signals. Here, we introduce a technique called photochemically induced dynamic nuclear polarization (photo-CIDNP) and discuss its progresses in enhancing the solution-state NMR sensitivity.

Recent NMR developments for pharmaceutical research

  • Lee, Kwanghwan
    • Journal of the Korean Magnetic Resonance Society
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    • v.20 no.1
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    • pp.27-35
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    • 2016
  • NMR spectrometer has been regarded as essential tool for structure elucidation in variable scientific field as like organic synthesis, natural product and macro protein research. Also NMR can be applied for defining dynamic behavior like ligand and receptor binding. One of advantage of research with NMR is that to be great confident to confirm structure and the measured sample could be recovered. Nevertheless NMR also has a weak points than other spectroscopic methods that require a lot of time for interpreting acquired spectrum and running time due to low sensitivity. For last two decade Bruker has developed hardware and software solution for overcome those weak points. In order to overcome low sensitivity Bruker introduced Cryo and Micro diameter probe head technology. And researcher can reduce the time for routine spectrum processing and interpretation works due to lots of introductions in software solutions for quantification, identification and statistics analysis. With four examples, this article describing those new hardware and software solutions in field of recent pharmaceutical research as follows. - New Horizons for NMR in the Biopharmaceutical Industry - The development and application of solid-state NMR spectroscopy (SSNMR) in pharmaceutical analysis - Assisted NMR Data Interpretation in Synthetic Chemistry - Complete Analysis of New Psychoactive Substances Using NMR.

Efficient baseline suppression via TIP and modified DEPTH

  • Hyun, Namgoong
    • Journal of the Korean Magnetic Resonance Society
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    • v.26 no.4
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    • pp.51-58
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    • 2022
  • The baseline flattened NMR spectrum has been achieved by several methodologies including pulse manipulation with a series of phase cycling. The background signal inherent in the probe is also main source of baseline distortion both in solution and solid NMR. The simple direct polarization with 90° pulse flipping the magnetization from the z-axis onto the receiver coil requires the strong rf pulse enough to encompass the wide frequency range to excite the resonance of interest nuclei. Albeit the perfect polarization 90° pulse, the signal from the unwanted magnetic fields such as background signal can not be completely suppressed by suitable phase cycling. Moreover, slowly baseline wiggling signal from the low 𝛾 nuclei is not easy to eliminate with multiple pulse manipulation. So there is still need to contrive the new scheme for that purpose in an adroit manner. In this article new triple pulse excitation schemes for TIP and modified DEPTH pulse sequence are analytically examined in terms of arbitrary phase and flip angle of pulse. The suitable phase cycling for these pulse trains is necessary for the good sensitivity and resolution of the spectrum. It is observed that the 13C sensitivity TIP experiment is almost equal to the CP/MAS with modified DEPTH sequence, both of which are applicable to both solid and solution state NMR.

High-pressure NMR analysis on Escherichia coli IscU

  • Jongbum Na;Jinbeom Si;Jin Hae Kim
    • Journal of the Korean Magnetic Resonance Society
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    • v.28 no.1
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    • pp.1-5
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    • 2024
  • IscU, the iron-sulfur (Fe-S) cluster scaffold protein, is an essential protein for biogenesis of Fe-S clusters. Previous studies showed that IscU manifests a metamorphic structural feature; at least two structural states, namely the structured state (S-state) and the disordered state (D-state), interconverting in a physiological condition, was observed. Moreover, subsequent studies demonstrated that the metamorphic flexibility of IscU is important for its Fe-S cluster assembly activity as well as for an efficient interaction with various partner proteins. Although solution nuclear magnetic resonance (NMR) spectroscopy has been a useful tool to investigate this protein, the detailed molecular mechanism that sustains the structural heterogeneity of IscU is still unclear. To tackle this issue, we applied a high-pressure NMR (HP-NMR) technique to the IscU variant, IscU(I8K), which shows an increased population of the S-state. We found that the equilibrium between the S- and D-state was significantly perturbed by pressure application, and the specific regions of IscU exhibited more sensitivity to pressure than the other regions. Our results provide novel insights to appreciate the dynamic behaviors of IscU and the related versatile functionality.

Nonlinear effects in solution NMR: A numerical study on dynamics of dipolar demagnetizing field and radiation damping

  • Sangdoo Ahn;Lee, Sanghyuk
    • Journal of the Korean Magnetic Resonance Society
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    • v.3 no.2
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    • pp.71-83
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    • 1999
  • The dynamics of the dipolar demagnetizing field is investigated by numerical simulation. The effects of radiation damping, molecular diffusion, and relaxation processes on the dipolar demagnetizing field are examined in terms of the modulation pattern of the z-magnetization and the signal intensity variation. Simulations for multi-components suggest applications for sensitivity enhancement in favorable conditions.

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The Study on the Synthesis of Propellant with High Nitrogen Content (고질소 추진물질 합성 연구)

  • Lee, Woonghee;Kim, Minjun;Park, Youngchul
    • Journal of the Korean Society of Propulsion Engineers
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    • v.19 no.3
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    • pp.96-102
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    • 2015
  • Traditional propellants emit toxic gases such as carbon dioxide and hydrogen chloride during combustion which are harmful to the environment. This study established a synthetic process of a high nitrogen containing derivative of tetrazine, 3,3-Azobis(6-Amino-1,2,4,5-Tetrazine) (DAAT), which can be applied as solid fuels for a solution to environmental concerns. Also, this paper described the detailed process and the analytic results of properties, which were not mentioned in previous reports. The compound was characterized by NMR, IR spectroscopy, and thermal, impact, and friction stability were measured. In addition, the heats of formation (${\Delta}H_f$) and detonation properties (pressure and velocity) of DAAT were calculated using Gaussian 09 and EXPLO5 programs.

Preparation of Polymeric Metal Complex Containing Azo Dye Rotaxane

  • Kang, Won-Young;Park, Jong-S.
    • Textile Coloration and Finishing
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    • v.23 no.3
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    • pp.163-168
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    • 2011
  • In this article, we synthesized an azo dye rotaxane containing bis(8-hydroxyquinoline) group and its polymeric metal complex with zinc. The azo dye rotaxane exhibits high pH sensitivity, solvatochromism and zinc (II) ion sensings in aqueous solution. These behaviors came from the tautomeric equilibrium between azo-hydrazone tautomers and the formation of extended conjugation. The structure of polymeric zinc complexed dye rotaxane was confirmed with NMR and FT-IR measurements. The existence of CD rings, provided by dye rotaxane formation, was found to be very beneficial in improving aqueous solubility of polymeric metal complex.

Synthesis and Photosensitive Properties of Poly[N-(formyloxyphenyl)maleimide] Containing Photosensitive Groups (Poly[N-(formyloxyphenyl)maleimide] 고분자의 합성과 자외선에 대한 반응특성)

  • Kim, Sang-Min
    • KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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    • v.10 no.1
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    • pp.55-62
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    • 2004
  • Synthesis of poly[N-(formyloxyphenyl)maleimide](PFOMI) as photopolymer were investigated with various kinds of photosensitive groups. Generally, photopolyimide have some deficiencies in solubility, sensitivity, reserve stability of the photosensitive solution, and the precision of image pattern. The study has been required on those polymers which have high glass transition temperature and photo efficiency, and low dielectricity. The existing condensation resins require high curing temperature and perfect elimination of subreacted materials that are produced during the process after irradiation and various membrane damages such as the deformation and contraction in image pattern cure. In this study poly[N-(hydroxyphenyl)maleimide](PHPMI) was synthesized. The PHPMI were analyzed by H-NMR and FT-IR. The measured number average molecular weight of PHPMI was produced was $1.06{\times}10^4$. Poly[N-(formyloxyphenyl)maleimide](PFOMI) as a type of photo-Fries rearrangement was synthesized by NHPMI and formic acid followed by radical polymerization. PFOMI was analyzed by FT-IR, and photocharacteristics was investgated by UV spectra and FT-IR before and after UV irradiation. Based on the image characteristics of PFOMI measured from optical micrographs, it was formed that the resolution of positive type PFOMI was $0.5{\mu}m$.

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Study on the History of Printing Culture - The Center of Jin-Ju Areas - (인쇄문화사에 대한 고찰 - 진주지역을 중심으로)

  • ChuNamJang
    • Journal of the Korean Graphic Arts Communication Society
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    • v.13 no.2
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    • pp.47-53
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    • 1995
  • Photosensitive resin of azide type is good for resolution and inner solvent, but it is really problem to development of practical use because fanctional groups of polymer has many hydrophilic radicals. By careful attention to this point, this study was investigated synthesis term, photo property and development property of composed photosensitive resin of azida type, it is to this effect. 1) H-NMR spectrum of compared DABCI showed amion redical by $\delta$6.0~6.1ppm to substitude for azide radical by amino radical by $\delta$8.9~9.45ppm, and FT-IR absorption spectra showed the absorption bends at 2100cm. 2)FT-IR absorption spectra of PHS1-DAB, PHS2-DAB, CMM-DAB and CHM-DAB showed azida radical pick to be lost at after irradiation by UV light. 3) According to exposuer change of PHS1-DAB, PHS2-DAB, CMM-DAB and CHM-DAB, absorption maximum value of UV spectrum change was 280nm. 4) to compared relative sensitivity of compared photosensitive resin, PHS2-DAB was the best and to compared insolubility rate of compared photosensitive resin, CMM-DAB was the lower. 5)Solubility if NaOH was the best by 1.0mol/$\ell$ and solubility of developing solution of ethanol to water was it in the ratio of 4 to 1.

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Positive-Type Photosensitive Polyimide Based on a Photobase Generator Containing Oxime-Urethane Groups as a Photosensitive Compound

  • Jang Young-Min;Seo Ji-Young;Chae Kyu-Ho;Yi Mi-Hye
    • Macromolecular Research
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    • v.14 no.3
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    • pp.300-305
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    • 2006
  • The chemical structure of a semi-aromatic polyimide-I, which was prepared by the chemical imidization of cyclopentanetetracarboxylic dianhydride and 2,2-bis(4-aminophenyl)hexafluoropropane, was characterized by $^{13}C-NMR$ spectroscopy. The chemically imidized polyimide-I was used for the preparation of a photosensitive polyimide (PSPI) through the addition of benzophenone and benzophenone oxime hexamethylene diurethane (BOHD), a photobase generator containing oxime-urethane groups. The polyimide-I film containing benzophenone and BOHD was not soluble in 2.38 wt% tetrabutylammonium hydroxide solution in $H_2O$. However, it became soluble following irradiation with 310 nm UV light. A positive tone image with a resolution of $5{\mu}m$ was obtained with this PSPI, having sensitivity($D_c$) of $1.2J/cm^2$ and contrast(${\gamma}_p$) of 1.08. Thus, a polyimide, which is not intrinsically photosensitive, can become photosensitive through the addition of a photobase generator containing oxime-urethane groups as a photosensitive compound.