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Chinese Journal of
Magnetic Resonance
(Quarterly, Started in 1983)
Editor-in-Chief: LIU Mai-li
Sponsored by
Wuhan Institute of Physics and Mathematics, CAS
Published by Science Press, China
Distribution Code: 38-313
Pricing: ¥ 80.00 per year
Current Issue
       Volume 20 Issue 1, 05 March 2003 Previous Issue   Next Issue
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      THE STRUCTURE OF A MPEG-b-PLA DIBLOCK COPOLYMERIN ITS SOLID PHASE STUDIED BY SOLID STATE NMR
    WU Guo-lin, SUN Ping-chuan, ZHANG Guo-lin, MA Jian-biao*
    Chinese Journal of Magnetic Resonance, 2003, 20(1): 1-7.  
    Abstract     HTML ( )   PDF(883KB)

    In this work, the structure of a poly(ethylene glycol) methyl ether-b- poly(L-alanine) copolymer (MPEG-b-PLA) in its solid- state was studied by 13C CP/MAS, DP/MAS and spin lattice relaxation time T1 NMR experiments. The results revealed that the PEG blocks are crystallizable in the solid state of the diblock polymer, but the degree of crystallinity is considerably lower in the diblock polymer state than that in pure PEG. It was found that the PLA blocks is rigid not only because of the formation of a large number of α-helices and a small number of β-sheets as secondary structures, but also owing to PLA crystallinity in the solid state. The results also implied that Cβ is more mobile than Cα at room temperature, and the β-methyl group rotates freely around its axis.

     STUDY OF DIFFUSION COEFFICIENT DISTRIBUTION OFLIPOPROTEINS BY PULSE-FIELD-GRADIENT (PFG)-NMR
    CUI Yan-fang1,2, WEN Jian3, LIU Mai-li1*
    Chinese Journal of Magnetic Resonance, 2003, 20(1): 8-15.  
    Abstract     HTML ( )   PDF(753KB)
    Qualitative and quantitative analysis of major fractions of lipoproteins such as LDL, VLDL and HDL, has great values in many biomedical applications, for instance, in the diagnosis of liver diseases, heart diseases and cancer, and in diet management. A method of using a continuous distribution model of diffusion coefficient to characterize lipoproteins was developed in this study. Commercial samples of HDL, LDL and their mixtures at HDL∶LDL ratios of 2∶1 and 1∶1 were used to test the validity of this approach. The results showed that, with the samples studied, the continuous distribution model of diffusion coefficient resulted in good fitting to experimental data.
    PRECISE MEASUREMENTS OF 13C-1H DIPOLAR SPECTRA UNDER SLOW MAGIC ANGLE SPINNING
    SHEN Yi-min1~4, CHEN Shi-ming1*, LIU Wu-yang2, JIN Gui-dong1,HORII Fumilaka3
    Chinese Journal of Magnetic Resonance, 2003, 20(1): 17-21.  
    Abstract     HTML ( )   PDF(674KB)
    A 2D MAS NMR method has been presented for precise measurements of 13C-1H dipolar spectra. On the basis of the exact solution of a MAS FID in two-site exchange, the 13C-1H spectra can be used to analyze molecular motion in solids.
    THE COMPLEX SITES OF METAL IONS Cr3+, Mn2+ AND Fe3+ WITH FLUOROQUINOLONE ANTIMICROBIALS STUDIED BY NMR METHODS
    CHEN Liang, MU Li-xuan, XU Hao
    Chinese Journal of Magnetic Resonance, 2003, 20(1): 23-27.  
    Abstract     HTML ( )   PDF(656KB)

    By measuring 1H and 13C NMR signals and 1H spin-lattice relaxation time T1, we have studied the complexes formed between fluoroquinolone antimic
    robials and metal ions Cr3+, Mn2+ and Fe3+. The complex sites of the metal ions with fluoroquinolone antimicrobials were measured.

    19F NMR STUDY ON PERFLUOROHEPTANOIC ACID AND PERFLUOROOCTANOIC ACID
    DU Ding-zhun
    Chinese Journal of Magnetic Resonance, 2003, 20(1): 29-36.  
    Abstract     HTML ( )   PDF(793KB)

    Surfactants perfluoroheptanoic acid (PFHA) and perfluorooctanoic acid (PFOA) were studied in solvents 1,1,2-trifluorotrichloroethane (TFTCE) and n-pentanol (C5-OH) by 19F NMR. The spectra of both compounds in both solvents displayed only one set of time-averaged spectral peaks, indicating that molecular exchange rate between micelle and monomer is faster than NMR timescale. All 19F resonance observed were assigned. Within the concentration range studied, all 19F nuclei in PFHA had lower chemical shifts (upfield shift) in TFTCE than in C5-OH, indicating the existence of larger deshielding effects in C5-OH. When PFHA dissolved in C5-OH, the 19F nuclei in the α-CF2 group had the largest chemical shift (δ), those in the ε-CF2 and ω-CF3 groups had
     the smallest δ; and the 19F nuclei in the β- and δ-CF2 groups had chemical shifts in between. When dissolved in different solvents, the chemical shift differences (in TFTCE vs. in C5-OH) of the 19F nuclei in the α-CF2 and ω-CF3 groups of PFHA, which locate at the ends of the fluorocarbon chain, were larger than those of the other 19F nuclei. By plotting chemical shift vs. the inverse of its concentration (1/C), the critical micellar concentrations (cmc) of PFHA was obtained, and is the concentration where the δ-1/C relationship starts to deviate from a linear relationship. cmc of PFHA in C5-OH and in TFTCE calculated in this study were 0.0195 mol/L and 0.0406 mol/L, respectively. The cmc of PFOA in C5-OH measured was 0.0547 mol/L. Using the chemical shift vs. 1/C relationship of different 19F nuclei to calculate cmc resulted in different values, and this might be an advantage for determining cmc using this method. By comparing the δ vs. 1/C relationship obtained experimentally with that calculated by stimulation, equilibrium constant (K) and aggregation number (n) for PFOA in C5-OH were obtained, and were 21(mol/L)-(n-1) and 3.9, respectively.

    27Al3+ IONS IN CaO-Al2O3-SiO2 ALUMINOSILICATE GLASSES STUDIED BY MAS NMR
    LI Ru-bi1, XU Pei-cang, MO Xuan-xue2
    Chinese Journal of Magnetic Resonance, 2003, 20(1): 37-42.  
    Abstract     HTML ( )   PDF(692KB)

    In this study, the coordination structure of Al3+ in CaO-Al2O3-SiO2 aluminosilicate glasses (CAS) was studied using solid-state 27Al and 29Si magic-anglespinning NMR. The results showed that: 1). most Al3+ ions in CAS aluminosilicate glasses are present in the form of AlO4 tetrahedra, and act as networkforming ions. A small part of Al3+ ions exist as network-modifying cations in the forms of six-, five- and other- coordinated aluminum. 2). Onb/T is inversely proportional to η, where Onb/T is the number of non-bridge oxygen atom per tetrahedra, and η is the ratio of the number of tetrahedral Al3+ to the total number of Al3+ in the region of interest (ROI). The slope of the Onb/T vs.η relationship is influenced by γ, where γ is the ratio of the total number of Al3+ to the total number of Si4+ in the ROI.

    A NMR STUDY ON PLANT CYCLOPEPTIDE DRYMARIN B
    TENG Rong-wei, DING Zhong-tao, HE Yi-neng, YANG Cong-ren, WANG De-zu*
    Chinese Journal of Magnetic Resonance, 2003, 20(1): 43-50.  
    Abstract     HTML ( )   PDF(852KB)

    Object  ]Severe spectral overlap often occurs in the 1H and 13C NMR spectra of plant cyclopeptides because of the similarity in chemical shifts of different amino acid residuals.  This paper aims to look for suitable NMR techniques for structural elucidation of plant cyclopeptides. Methods 2D NMR techniques such as  HMQC, HMBC, ROESY, and HMQC-TOCSY were used to study the structure of Drymarin B, a cyclopeptide isolated from the plant Drymaria diandra B1 (Caryophyllaceae).  Results  The 1H and 13C chemical shifts of the amino acid residuals (except for the quaternary carbons) can be assigned simultaneously using 2D HMQC-TOCSY  because this technique provides not only total proton correlation in the  F2 dimension but also total carbon correlation (except for the quaternary carbons) in the F1 dimension. The linkages among the anino acid residuals can be determined by  long range correlations from the HMBC spectra or NOEs from the ROESY or NOESY spectra. Conclusion   The 2D NMR techniques are  efficient tools for structural elucidation of plant cyclopeptides.

    DESIGNING DIGITAL NUCLEAR QUADRUPOLE RESONANCE SPECTROMETER BASED ON SOFRTWARE RADIO TECHNIQUE
    YANG Wen-hui, WANG Hui-xian, WANG Zhen
    Chinese Journal of Magnetic Resonance, 2003, 20(1): 51-56.  
    Abstract     HTML ( )   PDF(790KB)

    The basic principles of the software radio technique were introduced. The acquirements for designing a digital nuclear quadrupole resonance spectromet
    er were analyzed. Some considerations on using the software radio technique in designing a spectrometer, and particularly a digital nuclear quadrupole resonance spectrometer, were discussed.

    PERMEABILITY OF SANDSTONE MEASURED BY NMR RELAXATION METHOD
    WANG Li-jin, ZHOU Shang-wen, ZHOU Da-ming, GUO Zhen-ya, DING Da-tong
    Chinese Journal of Magnetic Resonance, 2003, 20(1): 57-61.  
    Abstract     HTML ( )   PDF(626KB)

    Based on a previous study on the absorption mechanisms of liquids in oil reservoir core, a method for determining the effective permeability of sandst
    one was developed in this study, and the results obtained appeared relatively satisfactory. The effective permeability of sandstone determined by this method was closer to the real value than that obtained by the conventional method. The value of effective permeability derived can be used for evaluating the performance/cost ratio of using the water flooding method in an oil field, and for studying the distribution of surplus oil in an oil field. It is believed that this method will find many practical applications.

    1H AND 13C NMR STUDY OF NATURAL RUBBER USING A HIGH RESOLUTION MAGIC ANGLE SPINNING PROBE: A COMPARISON STUDY
    WANG Xiao-jun, YUAN Zhi, ZHU Cheng-fei
    Chinese Journal of Magnetic Resonance, 2003, 20(1): 63-69.  
    Abstract     HTML ( )   PDF(730KB)

    1D/2D 1H and 13C NMR spectra of solid natural rubber, natural rubber latex and dissolved natural rubber in liquid phase were acquired using a BRUKER high-resolution magic angle spinning (HR/MAS) probe, a BRUKER solution broad bore (BBO) probe and a BRUKER solid CP/MAS probe. The results obtained from the three probes were compared. The results showed that high resolution 1H and 13C spectra could be obtained for solid nature rubber and rubber latex by using the HR/MAS probe, suggesting that the HR/MAS probe, in terms of signal-to-noise ratio and signal line width, is more advantageous than the CP/MAS probe for NMR studies on solid natural rubber.

    A 13C NMR STUDY OF ARYL α-NAPHTHYLACETYLAMIDES
    XU Yong-ting, LI Ying-jun, HU Jie-han, AN Yue
    Chinese Journal of Magnetic Resonance, 2003, 20(1): 71-73.  
    Abstract     HTML ( )   PDF(619KB)

    13C NMR spectra were acquired for 5 new aryl α-naphthylacetylamides we synthesized, which can potentially be used as plant growth regulators, anti-tumor medicine and chemical picking agent for fruits. By analyzing the 13C NMR spectra, the structures of the compounds were determined. The effects of hemical structures on the 13C chemical shifts in aryl α-naphthylacetylamides were discussed.

    AN OUTLINE OF NMR STUDIES OF DNA
    MAO Xi-an
    Chinese Journal of Magnetic Resonance, 2003, 20(1): 75-90.  
    Abstract     HTML ( )   PDF(907KB)

    Applications of NMR to the studies of DNA structures and dynamics are reviewed in aspects regarding NMR peak assignment, NMR constraints and structure calculation, main features of DNA NMR spectra, ring current effect on DNA chemical shifts, and DNA dynamics in solution. Unsolved problems in DNA NMR studies are also pointed out, which include: (1) The dihedral angle parameters in molecular modeling force field are not consistent with those in irregular DNA. (2) DNA structures simulated by molecular modeling usually do not have good consistency. (3) The ring current theory for explaining DNA chemical shifts is yet not ready for use. (4) The “modelfree” model has difficulties in interpreting steady-state NOE. Nonetheless, the structural and dynamical information provided by NMR is still important, and has greatly deepened our understanding of DNA.

    THE TECHNIQUE OF TIME RESOLVED CHEMICALLY INDUCED DYNAMIC POLARIZATION (CIDNP)
    GUO Xiao-yong, YAN Bao-zhen, GUO Hong-ling, TIAN Qiu1, LIU Yang
    Chinese Journal of Magnetic Resonance, 2003, 20(1): 91-100.  
    Abstract     HTML ( )   PDF(865KB)

    The general situation, principles, experimental aspects and applications of time-resolved chemically induced dynamic polarization (CIDNP) is briefly reviewed.

    IMPROVED RESOLUTION WITH SYMMETRICALLY SHIFTED PULSES—IMPRESS HMBC
    Ron Crouch
    Chinese Journal of Magnetic Resonance, 2003, 20(1): 101-104.  
    Abstract     HTML ( )   PDF(684KB)
    2D heteronuclear NMR experiments are very useful tools for determining the structure of small or medium molecules. Especially, the heteronuclear long
    -range experiments from 1H to 13C or 15N  are the most powerful implements to allow chemist the bridging of isolated fragments molecules and allow placement of quaternary 13C (or 15N) atoms. However, the resolution in the dimension of the heteroatom of indirect detection experiments can not meet the requirement of resonance assignment. Linear prediction, band-selection, and careful aliasing are three different strategies to achieve higher resolution. Recently a new approach has been advanced by utilizing Hadamard Excitation Sculpting. The high rf quality and flexibility of VNMR software tools allow users of Varian NMR systems to easily adopt novel excitation sculpting schemes to dramatically increase in gHMBC experiments.