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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 34 Issue 1, 05 March 2017 Previous Issue   Next Issue
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    Expression,Purification and Characterization of the Zinc-Finger (4-5) Domain in Human Protein INSM1   Collect
    WANG Hua-pu, ZHU Qin-jun, LIU Mai-li, YANG Yun-huang, YUE Xia-li
    Chinese Journal of Magnetic Resonance, 2017, 34(1): 1-7.   DOI: 10.11938/cjmr20170101
    Abstract     HTML ( )   PDF(781KB)
    Human insulinoma-associated protein 1 (INSM1) is a transcriptional regulator recognizing sequence-specific DNA through its C-terminal zinc finger (ZF) domains. INSM1 contains five zinc finger domains, whose structures are still not known; therefore, the mechanisms through which it recognizes DNA also remain unclear. In this study, we designed the recombinant plasmid pET-32m-INSM1(424-497), which can express the truncated INSM1 fragment containing the zinc finger domains 4 and 5[i.e., ZF(4-5)]. Expression and purification of ZF(4-5) were explored in order to achieve high protein yield for further structural and functional study. Nuclear magnetic resonance (NMR) and circular dichroism (CD) spectra revealed that chelation of Zn2+ to C2H2 in the ZF(4-5) was important for its structural stability, and also confirmed that the active-sites, Zn2+-chelated histidines, had the δ-tautomeric form.
    Determination of Aromatic Carbon Mole Ratio in Oil Samples by Quantitative 13C NMR Spectroscopy with DFSS Methodology   Collect
    MA Lin-ge, LONG Yin-hua
    Chinese Journal of Magnetic Resonance, 2017, 34(1): 8-15.   DOI: 10.11938/cjmr20170102
    Abstract     HTML ( )   PDF(253KB)
    Aromatic carbon mole ratios[C(ar)%] in model oil samples, which consisted of 11 saturated/unsaturated compounds with known contents, were determined by quantitative carbon nuclear magnetic resonance spectroscopy (13C qNMR) with the design for six Sigma (DFSS) methodology. An empirical model was established between C(ar)% and sample parameters, including sample concentration (Conc.), concentration of relaxation reagent Cr(acac)3 and relaxation delay (D1). Based on the model, the optimal condition was determined to be at sample concentration 180 mg/mL, concentration of Cr(acac)3 12 mg/mL and D1 10.5 s. Eight verification experiments were performed under the optimal condition, and the results showed fairly good repeatability (RSD=0.61%) and accuracy (99.0%~100.6%). The work also gave some supplementary suggestions on parameter settings for the current GB method/ASTM method.
    Interactions Between NP-10 and Single/Double Chain Quaternary Ammonium Salts Studied by NMR Spectroscopy   Collect
    MA Er-qian, LI Yong-xiao, ZHAO Rui-ge, ZHANG Zhan-hui, YANG Qiu-qing
    Chinese Journal of Magnetic Resonance, 2017, 34(1): 16-24.   DOI: 10.11938/cjmr20170103
    Abstract     HTML ( )   PDF(448KB)
    NMR spectroscopy was used to study the behaviors of three binary surfactant micellar solutions, NP-10/DTAC, NP-10/C12-C4-C12 and NP-10/C12-C8-C12 respectively. Relative arrangement and the sites of interactions between the surfactant molecule pairs in the mixed micelles, as well as the differences in inter-/intra- molecular interactions were investigated. 2D NOESY experiments revealed that the number of sites of interaction varied across the different binary mixtures, and the degree of interactions increased in the following order:NP-10/C12-C8-C12 > NP-10/C12-C4-C12 > NP-10/DTAC. Self-diffusion coefficient experiments showed that the influence of NP-10 on the hydro-dynamic radius of the mixed micelles was greater than that of quaternary ammonium salts. Spin-spin relaxation time experiments indicated that, for NP-10/DTAC and NP-10/C12-Cs-C12 (s=4 or 8) binary systems, intra-molecular interactions dominated and inter-molecular interactions began to decrease at molar ratios 1:3 and 1:2. These points corresponded to the optimal molar ratio for synergic effects. Spatial distance measurements supported this result, confirmed that the optimal molar ratio was 1:3 and 1:2.
    An NMR Study of a Novel N-Acylhydrazone Derivative Containing Benzimidazole Moiety   Collect
    LI Ying-jun, LI Ji-yang, JIN Kun, CAO Xin
    Chinese Journal of Magnetic Resonance, 2017, 34(1): 25-34.   DOI: 10.11938/cjmr20170104
    Abstract     HTML ( )   PDF(573KB)
    With 1D NMR, 2D NMR and variable-temperature 1H NMR, the 1H and 13C NMR chemical shift of two isomers (E/trans and E/cis) of a new N-acylhydrazone derivative containing benzimidazole moiety (new compound 1), naming 2-[2-(4-methylphenoxymethyl)-1H-benzimidazol-1-yl]-N'-{[4-(dimetilamino)phenyl]methylene}acetohydrazide, were assigned. Coupling constants and tautomeric ratios of the isomers were determined. Experimental results showed that compound 1 in DMSO-d6 had both E/trans and E/cis isomers, and the ratio of the dominant E/cis isomer was 74.2%.
    Spectral Analysis and Structural Elucidation of Triptophnolide   Collect
    WANG Fei-fei, ZHANG Yu-mei, HE Yi, DAI Zhong, MA Shuang-cheng, LIU Bin
    Chinese Journal of Magnetic Resonance, 2017, 34(1): 35-42.   DOI: 10.11938/cjmr20170105
    Abstract     HTML ( )   PDF(246KB)
    Ultraviolet (UV) spectrum, infrared (IR) spectrum, mass (MS) spectra and nuclear magnetic resonance (NMR) spectra (i.e., 1H NMR, 13C NMR, DEPT, 1H-1H COSY, NOE, 1H-13C HSQC and 1H-13C HMBC) of Triptophnolide were collected and interpreted. All 1H and 13C NMR signals were assigned. Base on the data, the structure of reference standard Triptophnolide was determined.
    Spectral Analysis of Bortezomib   Collect
    FENG Xiao-hu, YU Shui-tao, XIA Zheng-jun, CHEN Zai-xin
    Chinese Journal of Magnetic Resonance, 2017, 34(1): 43-51.   DOI: 10.11938/cjmr20170106
    Abstract     HTML ( )   PDF(433KB)
    Ultraviolet (UV) spectrum, infrared (IR) spectrum, electrospray ionization-mass spectra (ESI-MS) and nuclear magnetic resonance (NMR) spectra (i.e., 1H NMR, 13C NMR, DEPT, 1H-1H COSY, 1H-13C HSQC and 1H-13C HMBC) of bortezomib were collected and interpreted. All 1H and 13C NMR signals were assigned. The structure of the compound was preliminarily determined.
    Structure Elucidation of Taxol Based on Two-Dimensional NMR Spectra Collected on a 500 MHz NMR Spectrometer Built In-House   Collect
    ZHOU Qi, HUANG Chong-yang, GAO Shan, WANG Hui-juan, FENG Ji-wen, LIU Chao-yang, ZHANG Jin-zhi, ZOU Qi-chao
    Chinese Journal of Magnetic Resonance, 2017, 34(1): 52-60.   DOI: 10.11938/cjmr20170107
    Abstract     HTML ( )   PDF(443KB)
    A 500 MHz NMR spectrometer was successfully built in-house in Wuhan Institute of Physics and Mathematics in 2006, and it had been used for researches in many areas. However, the performance of this spectrometer in acquiring two-dimensional (2D) NMR spectra needed for structure elucidation had not been evaluated until now. In this paper, we acquired all the one-dimensional (1D) and 2D (i.e., 1H-1H COSY, 1H-1H TOCSY, J-Res, 1H-13C HMQC and 1H-13C HMBC) NMR spectra of taxol on this spectrometer, and used these spectra to elucidate the structure of the compound. The results showed that, with the spectra acquired on the 500 MHz NMR spectrometer built in-house, the structure of taxol could be elucidated correctly. We also corrected some incorrect NMR assignments of taxol existing in the literature.
    Application of 31P NMR in the Synthesis of Flame Retardant DOPO   Collect
    LAI Hua, LI Xiang, LIU Xing, ZHU Xiao-ming, TAN Xiong-wen, XIONG Ping-sheng
    Chinese Journal of Magnetic Resonance, 2017, 34(1): 61-68.   DOI: 10.11938/cjmr20170108
    Abstract     HTML ( )   PDF(380KB)
    The synthesis of flame retardant 9,10-dihydro-9-oxa-10-phosphaphen-anthrene-10-oxide (DOPO) involves many steps of chemical reactions, including esterification, Friedel-Crafts acylation, hydrolysis and dehydration. We analyzed the composition of the products from each of the steps with 31P NMR. The results were used to deduce the reaction routes and to optimize the reaction conditions. Based on the results, some key factors that may influence the yield and purity of DOPO were determined.
    Substituent Effects on the 1H NMR Chemical Shifts of CH=N(O) Bridge Group in Diaryl Nitrone   Collect
    CAO Chao-tun, LUO Qing-qing, CAO Chen-zhong
    Chinese Journal of Magnetic Resonance, 2017, 34(1): 69-77.   DOI: 10.11938/cjmr20170109
    Abstract     HTML ( )   PDF(362KB)
    A series of substituted diaryl nitrones XArCH=N(O)ArY were synthesized, and their 1H NMR spectra were measured. The 1H chemical shift of the CH=N(O) bridge groups, δH[CH=N(O)], in each compound was determined. The effects of substituents X and Y on δH[CH=N(O)] were investigated quantitatively. A four parameters correlation equation was constructed to model the changes of δH[CH=N(O)] with substituents, yielding a standard error of 0.020. The result indicated that δH[CH=N(O)] in substituted diaryl nitrones are mainly affected by four factors:field/inductive effect (S) of substituent X[σF(X)], conjugative effect of substituent Y[σR(X)], substituent specific cross-interaction effect between X and Y (Δσ2) and substituent specific crossinteraction effect between X and O-[Δσ2(X-O-)]. Among these factors, the contribution of Δσ2(X-O-) to δH[CH=N(O)] was more than 70%. A comparison of δH[CH=N(O)] in substituted diaryl nitrones to δH(CH=N) of the CH=N bridge group in diaryl Schiff base XArCH=NArY revealed no good linear relationship between δH[CH=N(O)] and δH(CH=N). Therefore it should be noted that one cannot simply use the change of δH(CH=N) to deduce the change of δH[CH=N(O)] when carrying out organic molecule structure elucidation with NMR spectra.
    Low-Field NMR Flowing Fluid Measurement: The Effects of Flow Rate and Corrections   Collect
    DENG Feng, XIAO Li-zhi, TAO Ye, GENG Dong-shi, WANG Meng-ying
    Chinese Journal of Magnetic Resonance, 2017, 34(1): 78-86.   DOI: 10.11938/cjmr20170110
    Abstract     HTML ( )   PDF(391KB)
    NMR measurement of flowing fluid is a highly effective and non-destructive online detection method, which can be widely used in pipeline fluid delivery process, chemical reaction process, river flowing process and other time-shift processes. However, flow will induce incomplete polarization and incomplete signal acquisition, such that the effects of flow rate on NMR measurement cannot be ignored. In this work, we analyzed quantitatively how factors related to the flowing state affect NMR measurement. Correction methods were proposed to achieve accurate NMR flowing fluid measurements.
    Design and Implementation of An Active Shimming System for Low Field NMR Analyzers   Collect
    CHEN Shan-shan, XIA Tian, BI Xin, MIAO Zhi-ying, YANG Pei-qiang, WANG Hong-zhi, DAI Shu-guang
    Chinese Journal of Magnetic Resonance, 2017, 34(1): 87-99.   DOI: 10.11938/cjmr20170111
    Abstract     HTML ( )   PDF(694KB)
    High homogeneity of the magnet field is an essential prerequisite for measuring weak signals and short spin-spin relaxation time on a nuclear magnetic resonance (NMR) analyzer. In this study, we designed active shimming coils, based on a target-field approach, for low filed NMR analyzers. Constant current source was designed according to the coil power supply. An active shimming platform used in a NMR analyzer's 0.45 T magnet system was constructed over a large target-diameter-sphere-volume (25.4 mm DSV) of interest. The basic structure and operation principles of the system, as well as the shimming method, were introduced. The feasibility and practicality of the design was demonstrated by experimental measurements.
    A Heterogeneous Dual-Core Receiver System for Magnetic Resonance Applications   Collect
    LIU Ying, ZHANG Yu-wen, LIANG Zhen, ZHANG Hao-wei
    Chinese Journal of Magnetic Resonance, 2017, 34(1): 100-107.   DOI: 10.11938/cjmr20170112
    Abstract     HTML ( )   PDF(805KB)
    A heterogeneous dual-core receiver system that combines advanced reduced instruction set computing (RISC) machines (ARM) and field programmable gate array (FPGA) is proposed for low-field nuclear magnetic resonance (NMR) applications. This system has advantages, such as high speed analog to digital converter (ADC) acquisition and variable gain control. In this design, the system generator, a system development tool from the Xilinx Company, can implement internal signal processing functions. Experimental results showed that, compared with the traditional receiver, the digital receiver had compact structure, strong reconstruction, high sampling rate and low cost. In addition, variable gain control enabled the digital receiver to achieve a large dynamic range such that the signal-to-noise ratio (SNR) of the reconstructed image could be improved.
    Determination of Treated and Control Wood on Fiber Saturation Point by Low-Field NMR Technology   Collect
    ZHOU Fan-ding, GAO Xin, CAI Jia-bin, ZHUANG Shou-zeng, ZHOU Hong-jie
    Chinese Journal of Magnetic Resonance, 2017, 34(1): 108-114.   DOI: 10.11938/cjmr20170113
    Abstract     HTML ( )   PDF(313KB)
    Due to its non-destructive characteristic, nuclear magnetic resonance (NMR) spectroscopy was used to study the fiber saturation point (FSP) of Pseudotsuga menziesii before and after heat treatment. The bound water amount in saturated wood cell wall was determined by analysis of T2 relaxation time distributions measured using GPMG (Carr-Purcell-Meiboom-Gill) sequence at -3℃ and 25℃. Results showed that the FSP of Pseudotsuga menziesii treated with various temperatures are 32.82% (180℃), 29.40% (200℃), 24.90% (220℃) and 38.76% (untreated), which indicate that FSP of Pseudotsuga menziesii decreases with increased heat treatment temperature. This study reflects that NMR could provide detailed information about wood water distribution rapidly and efficiently.
    Application of Solid-State NMR to Bone and Bone Biomaterials   Collect
    LI Dong-bei, XU Shuai, YU Zhi-wu
    Chinese Journal of Magnetic Resonance, 2017, 34(1): 115-129.   DOI: 10.11938/cjmr20170114
    Abstract     HTML ( )   PDF(883KB)
    Bone, as a structural organization and an important hematopoietic organ of the human body, plays critical biological roles in protecting human organs, storing calcium and phosphorus, participating in metabolism regulation and providing attachment sites for muscles. Understanding the microstructure of bone is important for intervention and treatment of bone diseases. However, experimental characterizations of the bone has been hindered by the morphological diversity of the bone, coexistence of organic and inorganic components, and sensitivity of bone samples to physical and chemical treatment. Compared with other techniques, solid-state nuclear magnetic resonance (NMR) can study the bone in-situ without any chemical pretreatment, thus avoiding changing bone structure. In addition, most of the chemical elements in the bone are magnetic resonance detectable, such as 1H, 13C, 31P, 19F, 43Ca, 29Si, 25Mg and 87Sr. Therefore, high resolution solid-state NMR technique provides a powerful tool for structural studies of the bone and bone biomaterials. In this paper, we reviewed the recent progresses in the application of solid-state NMR to bone and bone biomaterials studies.