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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 19 Issue 4, 05 December 2002 Previous Issue   Next Issue
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    L-BAND THREE DIMENSIONAL ESR IMAGING SYSTEM (Ⅰ)——Magnet and Magnetic Gradients for L-band 3D-ESRI
    WU Ke, CONG Jian-bo, XIAN Hong, WANG Chang-zhen, SUN Cun-pu, ZHENG Ying-guang, XU Jing, DONG Feng-xia, SHEN Er-zhong, XU Yu-shu, SONG Tao, HUANG Chang-gang, PEI Zhang-jing
    Chinese Journal of Magnetic Resonance, 2002, 19(4): 337-343.  
    Abstract     HTML ( )   PDF(4231KB)

    Main magnet, scan magnet and magnetic gradient coils used for L-band t hree dimensional electron paramagnetic resonance imaging were developed. Instead of using the conventional copper wire design to wind the gradient coils, they w ere built using a whole copper plate with the electrical line cut technique. The  new design remarkably reduced the volume of the gradient coils, and made the ma in magnet more effective. The maximum gradient strengths in all three directions  reached more than 200 mT/m with a driving current of 20 A. The spatial linearit y  of the gradients in all three directions was better than 5 %, and the linear ran g e was larger than a sphere of 42 mm in diameter. The distance between the surfac e s of the gradient coils was 63 mm, which was large enough to contain any type of   L-band EPR cavity. The main magnet and the scan magnet coils were fixed on an iron frame. The magnet fields generated by the two magnets were 1.6~96 mT (main  mag net) and 0.2~16 mT (scan magnet), respectively. All five magnet coils (main, sc an  and three gradients) were driven with five independent instant current power su pplies, which were controlled by a computer through a data interface. The prelim inary imaging test showed that the magnets are practical for 3D-EPRI applicatio ns.

    BENCH-TOP MAGNETIC RESONANCE IMAGING SYSTEM
    XIAO Peng-fei, SHEN Jie, JIANG Yun, JIANG Yu, LI Geng-ying*
    Chinese Journal of Magnetic Resonance, 2002, 19(4): 345-352.  
    Abstract     HTML ( )   PDF(899KB)

    Magnetic Resonance Imaging (MRI),as a non-invasive diagnosis method, has been widely used in many fields. However, students may have no chance to per form MRI experiments on commercial scanners, mainly due to the cost. In order to overcome this problem, we have constructed a bench-top MRI system in our labor a tory for teaching purposes. Detailed discussion about the system design is given  in this paper, including both hardware and software. The performance and reliab ility of our homebuilt bench-top MRI system were verified with some conventional MRI experiments. The results indicate that the system we designed can be used for educational applications.

    NMR STUDIES Of HARRINGTONINE INDUCED APOPTOSIS IN HL-60 CELLS
    WU Chang-lin1, QIAN Min2, HUANG Yong-ren1
    Chinese Journal of Magnetic Resonance, 2002, 19(4): 353-358.  
    Abstract     HTML ( )   PDF(686KB)

    NMR spectroscopy methods were used to study the metabolic changes of A TP, PME and lipid during harringtonine (HT) induced apoptosis in HL-60 cell. After HL-60 cells were treated with HT for two hours, it was observed by 31P-NMR sp ectroscopy that the levels of ATP and PME decreased significantly and intracellu lar pH increased significantly. It was also found by 1H-NMR a significa nt increa se in the signal intensity of methylene resonance and a slight decrease in choli ne peak in treated HL-60 cells. The present investigation will be helpful for  understanding the mechanism of Harringtonine induced apoptosis in HL-60 cells.

    CHARACTERIZATION OF REACTION-CARRYING SILOXANE ON THE SURFACE OF SILICA GEL BY NUCLEAR MAGNETIC RESONANCE SPECTROMETRY
    Chinese Journal of Magnetic Resonance, 2002, 19(4): 359-363.  
    Abstract     HTML ( )   PDF(749KB)

    The silica gel carried γ-chlopropyltrimethoxysilane and γ-aminopropyl trimethoxysilane were characterized by nuclear magnetic resonance spectrometry.  It was shown that the hydroxyl groups on the surface of silica gel substrate giv es only non-distinctive bands. The intensities of the bands related to the surface hydroxyl groups can be remarkably enhanced by cross polarization. The result  suggests that γ-chlopropyltrimethoxysilane and γ-aminopropyltrimethoxysilane  we recarried on the surface of the silicagel, and the reactions were relatively completed.

    A STUDY ON THE SYNTHESIS OF CEFAZOLIN COMPLEX WITH Eu3+ ION AND ITS COORDINATION SITES
    CHEN Liang, XU Hao, MU Li-xuan, LI Jing-xia
    Chinese Journal of Magnetic Resonance, 2002, 19(4): 365-370.  
    Abstract     HTML ( )   PDF(720KB)

    Cefazolin is an antibiotic, and sodium cefazolin is commonly known as  cephalexin. Solid complex of cefazolin with Eu3+ ion was synthesized in this study by the coprecipitation method. The complex synthesized was characterized by fluorescence spectroscopy, infrared spectroscopy (IR), thermal spectroscopy, scanning electron microscopic photographs and element analysis. The coordination sites of the complex and the mechanism of the complexing reaction were studied by  IR, 1H NMR and 13C NMR.

    31P NMR STUDIES OF INJURIES IN ERYTHROCYTES TREATED WITH METHYLENE BLUE PHOTOCHEMICAL METHOD
    WU Chang-lin1, LAN Rong2, LU Ping3, HUANG Yong-ren1
    Chinese Journal of Magnetic Resonance, 2002, 19(4): 371-376.  
    Abstract     HTML ( )   PDF(684KB)

    In order to understand injuries occurred in erythrocytes treated with  the methylene blue (MB) photochemical method, the changes of high-energy phosph a temetabolites in the treated erythrocytes were studied by 31P NMR. T he control and treated erythrocyte samples, which originally allcame from stored blood of  healthy adults, were measured by 31P NMR with an MSL-300 MHz spectr ometer. L-hist idine was added to half of the treated samples before the treatment. The effects  of the MB photochemical method on the erythrocytes were studied by measuring the relative changes of 2,3-DPG, ATP and (PME+SP) contents. In erythrocytes treat e d with MB photochemistry, the contents of (PME+SP) increased significantly, and  the contents of 2,3-DPG and ATP decreased significantly. Our data suggest that, in the MB treated erythrocytes, glucose metabolism through the pentose phosphate pathway increases significantly. It is concluded that MB treatment may affect physical, chemical and functional properties of erythrocytes to some degree, and such effects can be ameliorated by L-histidine.

    MICHAEL-TYPE ADDITION Of DBU WITH PERFLUORO ALKYNOATES AND NMR STUDIES OF THE PRODUCTS OF THE ADDITION REACTION
    Chinese Journal of Magnetic Resonance, 2002, 19(4): 377-384.  
    Abstract     HTML ( )   PDF(847KB)

    Reaction of 1,8-diazabicyclo\[5,4,0\] undec-7-ene (DBU)  with perfluoro- 2-alkynoates yielded tricyclic derivatives. The products were analyzed by 1H NMR,   13C NMR and 2D NMR spectroscopy. The resonances in 1H NMR and 13C NMR spectra  were assigned, and the structures of the products were determined. The pathways  and the mechanism of the addition reaction were also discussed.

    STUDY OF 17O-NMR CHEMICAL SHIFTS OF CHAINED ALIPHATIC ETHERS
    LI Li-dong, LI Lin-sheng*
    Chinese Journal of Magnetic Resonance, 2002, 19(4): 385-390.  
    Abstract     HTML ( )   PDF(626KB)

    Based on the results from five compounds: methylether, ethylether, n-propyleth er, em-propylether and t-butylether, an empirical equation: δcal=δ0n+Δα+Δβ+Δγ (Eq. [1]) was derived for calculating the 17O-NMR chemical shifts of  chained aliphatic ethers. Parameters were obtained for 29 substituents using lin ear regression in combination with least square analysis. The validity of Eq. [1] was checked regressively by 147 17O-NMR chemical shifts of 147 chained aliphat ic ethers. The confidence limit was 99.5 % and the calculating errors of about 9 0 % compounds were less than 5 ppm (relative errors 0.5 %).

    POLARIZABILITY EFFECT OF ALKYL GROUP ON 13C CHEMICAL SHIFT OF C=O
    QIAO Jie, LI Mei-ping, LU Fei, ZHANG Sheng-wan*
    Chinese Journal of Magnetic Resonance, 2002, 19(4): 391-394.  
    Abstract     HTML ( )   PDF(628KB)

    The relation between the 13C chemical shift of C=O in alkyl substitute d compound RXC=O and the polarizability effect index (PEI) of alkyl group R can  be expressed as
    δ=a+b·ΣPEI(R)
    where a and b are empirical constants. Regression analysis showed that the equat ion is a good expression for the 13C chemical shift of C=O change rule  with the  polarizabality effect index of alkyl group. The results also showed that the pol arizability effect index of alkyl group R increase the 13C chemical sh ift of C=O.

    STRUCTURE ELUCIDATION OF ELISABATIN B WITH QUATERNARY CARBONS BY 2D NMR SPECTROSCOPY
    SHI Yan-ping1, WU Qin-juan1, RODRIGUEZ Abimael D2
    Chinese Journal of Magnetic Resonance, 2002, 19(4): 395-400.  
    Abstract     HTML ( )   PDF(753KB)

    2D NMR (1H-1H COSY, HMQC and HMBC) methods, among which the HMBC metho d was the most important, were used to elucidate the structure of Elisabatin B ( i.e, diterpene with 11 quaternary carbons). The 1H and 13C chemi cal shifts were  assigned. Compared with the results reported in reference, the chemical sh if ts of 11 more quaternary carbons were determined. The results of this study sugg est that the 2D NMR techniques can be applied to and are useful in structural el ucidation of natural products.

    APPLICATION OF NMR IN STUDYING THE MECHANISM OF CHEMICAL REACTIONS INVOLVING FLUORINE -CONTAINING LACTONES
    Chinese Journal of Magnetic Resonance, 2002, 19(4): 401-408.  
    Abstract     HTML ( )   PDF(932KB)

    The fluorine-containing lactones are often present in natural organic- compounds. In this study the structures of three fluorine-containing lactones were determined using the NMR techniques(1H NMR,13C NMR,1H -1H COSY,NOESY,HMB C,HMQC). Two-dimensional NOESY was especially useful for providing information on the stereo configuration of the compounds. Knowing the structures can be help ful in studying the mechanism of chemical reactions involving fluorine-containi ng lactones.

    CHARACTERIZATION OF INDOLE DERIVATIVES BY 1H-1H COSY SPECTROSCOPY
    ZHOU Yong, YAO Xia-jun, YUN Liu-hong
    Chinese Journal of Magnetic Resonance, 2002, 19(4): 409-413.  
    Abstract     HTML ( )   PDF(739KB)

    Indole derivatives are important pharmaceutical compounds often used for anti-anxiety treatments. In this study, the structures of a serials of indole based co mpounds were determined by 1H, 1H-1H COSY, MSFAB, IR and ele ment analysis. The 1H chemical shifts of the compounds were assigned. The  positions of the substitute groups were determined by 1H-1H COSY. The 1H chemical shifts of different indole derivatives were compared.

    MEASUREMENT OF CHEMICAL SHIELDING TENSOR
    WANG Li-ying, DENG Feng, YE Chao-hui*
    Chinese Journal of Magnetic Resonance, 2002, 19(4): 415-445.  
    Abstract     HTML ( )   PDF(2034KB)

    In rigid lattice, chemical shift is a tensor depending on the spatial orientation of the external magnetic field. The tensor has six independent components. The  orientation of chemical shielding tensor can be expressed with direction cosine s of its principal axis system. It is of great interest that if the chemical shi ft tensor of each nonmagnetically equivalent nucleus is known, the information o n the distribution of the electron cloud in the molecule can be deduced from the se tensors. In this paper, the theory and methods of measurement of chemical shi ft tensor are reviewed. A number of common methods are discussed in detail, such  as 2D magic angle hopping (MAH), 2D magic angle turning(MAT), and 2D phase-adjusted spinning sidebands(2D-PASS) technique and so on. The common metho ds for measuring single crystal chemical shielding tensor are also discussed.

    APPLICATION OF CRYOGENIC NMR PROBES
    FENG Rui, XIE Hua, REN Da-zhou
    Chinese Journal of Magnetic Resonance, 2002, 19(4): 447-454.  
    Abstract     HTML ( )   PDF(845KB)
    In the past decade manufactures of NMR systems have put many efforts into the re search and development of new NMR probe technologies. Recently the development o f cryogenically cooled NMR probe has been the subject of considerable interest i n the light of the large sensitivity gains they may provide, and hence the savin gs in acquisition time by using this technology. For low gamma nuclides, such as 15N, the advantages that cryogenic NMR probes provide in terms of det ection sen sitivity and acquisition time may, in a sense more important than the enhancemen t of sensitivity per se, provide the opportunity of direct detection of NMR sign als in their natural abundances, while isotopeenriched samples often have to b e used when conventional NMR probes are employed. In this study, 5~10 Hz optimi ze d CIGAR-HMBC 1H-15N experiments were performed on a 2 mg natural a bundance sampl e of the oxazolidinone antibiotic eperezolid in a 3 mm NMR tube using a 5 mm Varian 1H-15N Cryo-QNMR probe and a 3 mm gradient inverse triple res onance probe,  and the results from the two probes were compared. With the cryogenic NMR probe, a 1H-15N CIGAR-HMBC spectrum, in which most previously reportedlong -range coup lings were observed, was recorded in ~10 min. Almost all of the expected long-r ange responses were observed when the acquisition time was increased to 26 min.  The same experiment using the conventional probe gave data that were of substant ially lower quality. About four hours were required for the conventional probe t o acquire a spectrum that displayed all the coupling responses as those shown by  the 26 min cryogenic probe spectrum. Eighteen hours of acquisition time were re quired for the conventional probe to obtain a spectrum that was comparable in terms of signal-to-noise ratio to that obtained by the cryogenic probe in 26 min.