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Overcoming the Challenges in Solution Structure Studies of CTG and CCTG Repeats
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Sik Lok Lam
Chinese Journal of Magnetic Resonance, 2012, 29(1): 1-20.
Genetic instability of deoxyribonucleic acid (DNA) repeating sequences has been found to associate with hereditary neurodegenerative diseases. It has been suggested that self-expansion of CTG and CCTG repeats would occur through the formation of unusual structures during DNA replication, leading to myotonic dystrophy type 1 (DM1) and myotonic dystrophy type 2 (DM2), respectively. Although x -ray crystallography is a powerful technique in solving DNA structures, there has not been any successful structure determination of CTG or CCTG repeats probably due to the fact that the growth of diffraction-quality crystals has been hampered by the intrinsic flexibility of these repeating sequences. Therefore, nuclear magnetic resonance (NMR) spectroscopy remains to be the only technique that allows studying DNA structures at individual residue level. Recently, we have successfully overcome the challenges in NMR structural studies of CTG and CCTG repeats, including the severe signal overlap due to the repetitive nature of repeating sequences and the increase in spectral complexity owing to the presence of multiple conformers and conformational exchange. With appropriate sample design, sample handling technique, sequence modification and/or single-site substitution experiments, we have determined the structural features of CTG and CCTG repeats using 1 H and 31 P NMR spectroscopy. This review provides an account of the strategies that have been applied in these studies.
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Analyses of Influencing Factors of Hydrocarbon Identification Using NMR Time Domain Analysis
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LI Yang, XIAO Li-Zhi, SUN Hua-Feng
Chinese Journal of Magnetic Resonance, 2012, 29(1): 21-31.
Time-domain analysis (TDA) is one of the most important NMR methods used in fluid identification and porosity calculation. It shows great advantages in reservoir evaluation, but there are also certain limitations. In order to investigate the adaptability of TDA in hydrocarbon identification under different reservoir conditions, numerical simulation was used in this study to analyze the factors influencing the outcomes of TDA, including longitudinal relaxation time T 1 , polarization time T W , porosity, hydrocarbon saturation, hydrogen index HI and polarization function. It is concluded that when acquisition mode D9TW is chosen, the viscosity of oil that can be measured by TDA is less than 9 mPa.s. After changing the short waiting time up to 2 s while keeping the long waiting time constant, the minimal viscosity reduces to less than 4 mPa.s. We also found the intensity of differential signals correlated positively with all the influencing factors mentioned above. With real low SNR NMR data, TDA can effectively identify hydrocarbon and calculate porosity only under the conditions that the differential porosities of hydrocarbon are greater than 1.5 p.u.
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A Novel Method for NMR Ringing Reduction under Downhole Condition
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HUANG Ke, XIAO Li-Zhi, LI Xin
Chinese Journal of Magnetic Resonance, 2012, 29(1): 42-50.
In NMR logging, the noise amplitude of ringing is often high, impacting echo signals detection. The phase-alternate pulse sequence (PAPS) technique is a conventional method to reduce NMR ringing. However, the amplitude of ringing is frequency-dependent, and the PAPS technique is effective at certain frequency, leading to a lower vertical resolution. Taking advantage of the feature that the echo signals change with the variation of RF pulse wherase the ringing noise keeps constant, we proposed a novel method, combining PAPS and stackingbetweenechoes, to reduce NMR ringing under downhole condition. The results showed that this method has improved efficiency. The echo train measured by the new method had the characters of high SNR and high vertical resolution compared to that measured by the PAPS technique, and the stacking between the echo trains was not limited to one frequency.
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Water Flooding Studied by Measuring NMR Two-Dimensional Distribution Function
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QU Yan-Tao, JIANG Zhi-Min, SHI Jing-Sheng, ZHU Tao-Tao, MENG Xiao-Hai, WANG Wei-Min
Chinese Journal of Magnetic Resonance, 2012, 29(1): 51-59.
The distribution of water and oil is a very important property of porous media such as rock cores. The study on water flooding is an essential part in the research of enhanced oil recovery (EOR). Nuclear magnetic resonance (NMR) diffusion-relaxation two-dimensional (2D) distribution function (spectrum) provides a large variety of information of fluids in porous media. Compared with NMR 1D relaxation spectrum, the 2D spectrum greatly improves the ability to separate water from oil. In this article, two sets of core flooding experiments were conducted. The relaxation spectra of water were extracted from the 2D spectra acquired with different oil saturations,and used to calculate wettability and distribution of water and oil in different pores under the condition of higher oil viscosity. It was shown that the difficulty of oil and water separation by traditional 1D NMR relaxation spectrum can be overcome by using the 2D method.
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Software System Design in an Integrated NMR Spectrometer Console
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SHANG Yun, ZHOU Juan, LEI Dou, XU Jun-Cheng, JIANG Yu
Chinese Journal of Magnetic Resonance, 2012, 29(1): 68-77.
The paper introduces the design of the software system in an integrated NMR spectrometer console. The software system is composed of two parts: the console software composed of embedded Linux operation system and real-time control software and the GUI control software in PC. The communication between the console and PC is achieved by network and programmed based on SOCKET such that the console can be controlled and updated in remote. The software system was tested by NMR experiments. This paper elaborates the design concepts and methods of the software system.
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A Preliminary Study on Field Distribution in a Slotted Tube Cavity
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KANG Song-Bai, LI Wen-Bing, ZHONG Da, MEI Gang-Hua
Chinese Journal of Magnetic Resonance, 2012, 29(1): 86-92.
Slotted tube cavity has been used in rubidium atomic frequency standards, but the microwave field distribution inside the cavity is unknown. Recently we calculated the microwave field distribution inside the cavity using high frequency structure simulation software (HFSS), and measured the field distribution experimentally with the optical-microwave double resonance method. The theoretical and experimental results were found consistent with each other. The results showed that magnetic lines of the microwave field lay along the cavity axis, impling that the cavity is suitable for applications in atomic frequency standards. The results also showed that the field distribution is spatially inhomogeneous, suggesting that the cavity needs to be improved further, since field inhomogeneity could affect the signal intensity of atomic clock transition.
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An NMR Study on Two Glucosylated Steroidal Saponins of Tb
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KANG Li-Ping, WANG Yong-Ze, FENG Bing, ZHOU Wen-Bin, XIONG Cheng-Qi, ZHAO Yang, TAN Da-Wei, LIU Chao, MA Bai-Ping
Chinese Journal of Magnetic Resonance, 2012, 29(1): 101-111.
Two glucosylated steroidal saponins of Tb were elucidated as pennogenin-3-O -α-D-glucopyranosyl-(1→3)-[α-L-rhamnopyranosyl-(1→2)]-β-D-glucopyranoside (1 ), and pennogenin-3-O -α-D-glucopyranosyl-(1→4)-α-D-glucopyranosyl-(1→3)-[α-L-rhamnopyranosyl-(1→2)]-β-D-glucopyrannoside (2 ) by MS, 1 H NMR, 13 C NMR, COSY, HSQC and HMBC analysis. 1 and 2 are new compounds. The 13 C and 1 H NMR chemical shifts of these two new compounds were assigned.
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2D NMR Assignments of an ent -Pimarane Diterpenoid from Euphorbia yinshanica
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ZHANG Ben-Yin, WANG Huan, LUO Xiao-Dong, DU Zhi-Zhi, SHEN Jian-Wei, ZHANG Xiao-Feng
Chinese Journal of Magnetic Resonance, 2012, 29(1): 112-118.
One known ent pimarane type diterpenoid, 3α, 19-dihydroxyl ent pimara- 9(11), 15-diene, has been isolated from the roots of Euphorbia yinshanica for the first time. Its structure has been confirmed by 2D spectral methods (1 H-1 H COSY, HMBC, HMQC, ROESY), and its NMR signals have been first completely assigned.
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Pure and Mixed Enantiomer of Moxifloxacin Hydrochloride Studied by NMR Spectroscopy
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YANG Qiu-Qing, LIU Bo-Qian, HAN Kang
Chinese Journal of Magnetic Resonance, 2012, 29(1): 119-127.
The structures of pure and mixed enantiomer of moxifloxacin hydrochloride were elucidated by NMR. The chemical shift of the spectral peaks were assigned using 1 H and 13 C NMR, COSY, HSQC, HMBC and 2D NOESY techniques, as well as 19 F-13 C coupled splitting. It was found that 19 F-13 C coupling exists not only in the sixmembered ring, but also in the fivemembered heterocyclic ring, and that 4 J FC in the five-membered heterocyclic ring is larger than 3 J FC and 4 J FC in the sixmembered ring. The spectral characteristics of the pure and mixed enantiomer of moxifloxacin hydrochloride were summarized. A method was proposed to differentiate the pure and mixed enantiomer of moxifloxacin hydrochloride.
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Analysis of Phytomedicines
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YU Hai-Yan, WU Xiang-Yu, ZHANG Li-Min, TANG Hui-Ru
Chinese Journal of Magnetic Resonance, 2012, 29(1): 128-141.
As widely used medicines in the world, phytomedicines played important roles in human health. The analysis of herbal medicines is important for the development of new drugs and functional food. Such analysis includes traditional methods, including metabolite extraction, component isolation and structure elucidation, and the hyphenated techniques with the combination of chromatographic and spectroscopic techniques. Here, we review the general procedures of traditional methods and hyphenated techniques for phytomedicine analysis with emphasis on the hyphenated HPLC-DAD-SPE-NMR-MS techniques.