• Title/Summary/Keyword: Solid-state NMR probe

Search Result 18, Processing Time 0.032 seconds

Solid-state NMR Studies of Membrane Proteins Using Phospholipid Bicelles

  • Kim, Yong-Ae
    • Bulletin of the Korean Chemical Society
    • /
    • v.27 no.3
    • /
    • pp.386-388
    • /
    • 2006
  • Membrane proteins in highly oriented lipid bilayer samples are useful for membrane protein structure determination. We used in the past planar lipid bilayers which were aligned and supported on the glass slide. These samples were mechanically aligned in a magnetic field. However, these stacks of glass slides with planar lipid bilayers are not well suited for use with a commercial solid-state NMR probe with a round coil. Therefore, a homebuilt solid-state NMR probe was built and used with a stack of thin glass plates wherein the RF coil was wrapped directly around the flat square sample. Recently, we began to use magnetically aligned bicelles that are suitable for the structure determination of membrane proteins by solid-state NMR spectroscopy without any effort to build a flat square coil probe. These bicelle samples are well suited for use with a commercial solidstate NMR probe with a round coil, are very easy to prepare and are very stable, so that they can be kept for more than a year. In this paper, we present the solid-state NMR spectra of optimized and magnetically oriented bicelle samples of membrane proteins.

Construction of 1H-15N Double Resonance Solid-State NMR Probe for Membrane Proteins in Aligned Bicelles

  • Park, Tae-Joon;Kim, Ji-Sun;Um, Seung-Hoon;Kim, Yong-Ae
    • Bulletin of the Korean Chemical Society
    • /
    • v.31 no.5
    • /
    • pp.1187-1191
    • /
    • 2010
  • $^1H-^{15}N$ heteronuclear dipolar coupling solid-state NMR experiments on lipid bilayer or bicelle samples are very useful for the structural studies of membrane proteins. However, to study these biological samples using solid-state NMR, a specific probe with high efficiency and high capability is required. In this paper, we describe the optimized design, construction, and efficiency of a 400 MHz wide-bore $^1H-^{15}N$ solid-state NMR probe with 5-mm solenoidal rf coil for high power, multi-pulse sequence experiments, such as 2D PISEMA or 2D SAMMY.

Home-built Solid-state NMR Probe for Membrane Protein Studies

  • Kim, Yong-Ae;Hwang, Jung-Hyun;Park, Jae-Joon
    • Bulletin of the Korean Chemical Society
    • /
    • v.24 no.9
    • /
    • pp.1281-1283
    • /
    • 2003
  • Proteins in highly oriented lipid bilayer samples are useful to study membrane protein structure determination. Planar lipid bilayers aligned and supported on glass slide were prepared. These stack of glass slide with planar lipid bilayers are not well fit for commercial solid-state NMR probe with round coil. Therefore, homebuilt solid-state NMR probe was built and used for a stack of thin glass plates and RF coil is wrapping directly around the flat square sample. The overall filling factor of the coil is much better and the large surface area enhances the extent to orientation by providing uniform environments for the phospholipids and the high ratio of circumference to area reduces edge effects. $^1H\;and\;^{15}N$ double resonance probe for 400 MHz NMR (9.4T) with a flat coil (coil size: 11 mm ${\times}$ 20 mm ${\times}$ 4 mm) is constructed and tested.

Low-ε Static Probe Development for 15N-1H Solid-state NMR Study of Membrane Proteins for an 800 MHz NB Magnet

  • Park, Tae-Joon;Choi, Sung-Sub;Jung, Ji-Ho;Park, Yu-Geun;Kim, Yongae
    • Bulletin of the Korean Chemical Society
    • /
    • v.34 no.3
    • /
    • pp.823-826
    • /
    • 2013
  • A low-${\varepsilon}$ solid-state NMR(Nuclear Magnetic Resonance) probe was developed for the spectroscopic analysis of two-dimensional $^{15}N-^1H$ heteronuclear dipolar coupling in dilute membrane proteins oriented in hydrated and dielectrically lossy lipid environments. The system employed a 800 MHz narrow-bore magnet. A solenoid coil strip shield was used to reduce deleterious RF sample heating by minimizing the conservative electric fields generated by the double-tuned resonator at high magnetic fields. The probe's design, construction, and performance in solid-state NMR experiments at high magnetic fields are described here. Such high-resolution solid-state NMR spectroscopic analysis of static oriented samples in hydrated phospholipid bilayers or bicelles could aid the structural analysis of dilute biological membrane proteins.

Developing 500 MHz NB 19F-13C Double Resonance Solid-State NMR Probe for in-situ Analysis of Liquid Crystal Display Panels

  • Choi, Sung-Sub;Jung, Ji-Ho;Park, Yu-Geun;Park, Tae-Joon;Park, Gregory Hyung-Jin;Kim, Yong-Ae
    • Bulletin of the Korean Chemical Society
    • /
    • v.33 no.5
    • /
    • pp.1577-1580
    • /
    • 2012
  • The orientational and dynamic behavior of liquid crystal molecules on the alignment layer surfaces of liquid crystal display (LCD) devices is crucial to their performance, but there are only a few methods of experimentally elucidating the interactions between the liquid crystals and the alignment layers. Inspired by the natural and technical similarities between membrane proteins in lipid bilayers and liquid crystals in LCDs, we employed solid-state NMR methodologies originally developed for the study of membrane proteins in lipid bilayers for the in-situ analysis of liquid crystal display panels. In this article, we present a home-built 500 MHz narrowbore (NB) The orientational and dynamic behavior of liquid crystal molecules on the alignment layer surfaces of liquid crystal display (LCD) devices is crucial to their performance, but there are only a few methods of experimentally elucidating the interactions between the liquid crystals and the alignment layers. Inspired by the natural and technical similarities between membrane proteins in lipid bilayers and liquid crystals in LCDs, we employed solid-state NMR methodologies originally developed for the study of membrane proteins in lipid bilayers for the in-situ analysis of liquid crystal display panels. In this article, we present a home-built 500 MHz narrowbore (NB) $^{19}F-^{13}C$ double resonance solid-state NMR probe with a flat-square coil and the first application of this probe for the in-situ analysis of LCD panel samples. double resonance solid-state NMR probe with a flat-square coil and the first application of this probe for the in-situ analysis of LCD panel samples.

Structural Studies of Membrane Protein by Solid-state NMR Spectroscopy (고체상 핵자기공명 분광법을 이용한 막단백질의 구조연구)

  • Kim, Yongae
    • Analytical Science and Technology
    • /
    • v.17 no.5
    • /
    • pp.388-392
    • /
    • 2004
  • Structural studies of membrane proteins, importantly involving interpretation of genomics information, many signaling pathway and major drug target for drug discovery, are having difficulty in characterizing the function using conventional solution nmr spectroscopy and x-ray crystallography because phospholipid bilayers hindered fast tumbling and crystallization. Here, we studied the structure of the pf1 coat protein in oriented phospholipid bilayers by home-built solid-state NMR probe. Bacteriophage pf1 was purified from Paeudomonas Aeruginosa and coat protein of bacteriophage pf1 was isolated from DNA and other proteins.

Construction of 19F-13C Solid-State NMR Probe for 400MHz Wide-Bore Magnet

  • Jeong, Ji-Ho;Park, Yu-Geun;Choi, Sung-Sub;Kim, Yongae
    • Journal of the Korean Magnetic Resonance Society
    • /
    • v.17 no.2
    • /
    • pp.81-85
    • /
    • 2013
  • Various fluorine-containing materials are used in electronic devices like LCD display panels and Li-ion batteries. The structural conformation of fluorine in fluorinated materials is an important contributing factor that influences the chemical and physical properties. The conformation can be changed by heat and stress during manufacture or use. Understanding the conformational changes is critical for understanding the performance and durability of electronic devices. Solid-state NMR spectroscopy could be widely used for the analysis of various fluorine-containing materials for electronic devices. However, conventional CPMAS probes cannot be used for in-situ analysis of fluorine-containing electronic devices like LCD panels and Li-ion batteries. In this paper, we show the design, construction, and optimization of a $^{19}F-^{13}C$ double-resonance solid-state NMR probe for a 400MHz wide-bore magnet with a flat square coil for in-situ analysis of fluorine-containing electronic devices without observing fluorine background signals. This custom-built probe does not show any fluorine background signals, and can have higher efficiency for lossy samples.

$^2D$ NMR Probe Development for Investigation of Biosupramolecular Systems

  • Kim, Andre;Kang, Shin-Won;Park, Jang-Su
    • Journal of the Korean Magnetic Resonance Society
    • /
    • v.8 no.1
    • /
    • pp.55-61
    • /
    • 2004
  • Biosupramolecular systems such as biological membranes usually fluid under physiological conditions$^1$. Therefore, solid-state NMR has been used to investigate biosupramolecular systems. But solid-state NMR spectra contain a large number of overlapping resonances and are rather difficult to analyze. These problem has to be overcome by selective isotope labeling. We constructed a deuterium NMR probe for AM400 NMR spectrometer, which is mainly used for liquid samples. To overcome the fluidity problem, a saddle type coil was designed. The efficiency was systematically investigated for two kinds of coil geometry, solenoid and saddle types. Our results suggest that solenoids are superior to saddle type coils in the sensitivity. However, the letter fits better to fluid samples such as biosupramolecular systems.

  • PDF

Development of 600-MHz 19F-7Li Solid-State NMR Probe for In-Situ Analysis of Lithium Ion Batteries

  • Jeong, Ji-Ho;Park, Yu-Geun;Choi, Sung-Sub;Kim, Yongae
    • Bulletin of the Korean Chemical Society
    • /
    • v.34 no.11
    • /
    • pp.3253-3256
    • /
    • 2013
  • Lithium is a highly attractive material for high-energy-concentration batteries, since it has low weight and high potential. Rechargeable lithium-ion batteries (LIBs), which have the extremely high gravimetric and volumetric energy densities, are currently the most preferable power sources for future electric vehicles and various portable electronic devices. In order to improve the efficiency and lifetime, new electrode compounds for lithium intercalation or insertion have been investigated for rechargeable batteries. Solid-state nuclear magnetic resonance (NMR) is a very useful tool to investigate the structural changes in electrode materials in actual working lithium-ion batteries. To detect the in-situ microstructural changes of electrode and electrolyte materials, $^7Li-^{19}F$ double-resonance solid-state NMR probe with a static solenoidal coil for a 600-MHz narrow-bore magnet was designed, constructed, and tested successfully.

Solid State NMR Studies of Proton Conducting Polymer, Poly(vinyl phosphonic) acid

  • Lee, Young-Joo;Bingol Bahar;Murakhtina Tatiana;Sebastiani Daniel;Ok, Jong-Hwa;Meyer Wolfgang H.;Wegner Gerhard;Spiess Hans Wolfgang
    • Proceedings of the Polymer Society of Korea Conference
    • /
    • 2006.10a
    • /
    • pp.347-347
    • /
    • 2006
  • Polymers containing poly(vinyl phosphonic) acid segments are promising candidates to be used as proton conducting membranes. Solid state NMR spectroscopy represents an ideal probe of proton motion on the molecular level, because it allows us to selectively detect the nuclei of interest. In this paper, we apply solid state NMR methods to poly(vinyl phosphonic) acid in order to demonstrate that the proton conduction of poly(vinyl phosphonic acid) results from P-OH proton through hydrogen bonding and that the condensation of phosphonic acid leads to decrease in proton conductivity. $^{1}H\;and\;^{31}P$ solid state NMR experiments are supported by quantum chemical computation of NMR parameters.

  • PDF