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Applications of Advanced Solid-State NMR Techniques in Studying the Structure and Dynamics of Polymers
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ZHANG Rong-Chun, SUN Ping-Chuan
Chinese Journal of Magnetic Resonance, 2012, 29(3): 307-338.
With the advances in NMR theories and spectrometer hardware technology, NMR is playing an increasingly important role in studying multiscale structure and dynamics of polymers. In this paper, the newest developments in solid-state 1 H and 13 C NMR techniques and their applications in the studies of polymer structures and dynamics were reviewed. High-resolution solid-state 1 H NMR techniques, such as multiple-pulse and fast magic angle spinning (MAS), have made it possible to determine the chemical structures of polymers and to detect the intra- and inter-polymer interactions effectively. Taking advantages of through-bond (J- coupling) and through-space (dipolar coupling) interactions, two dimensional heteronuclear correlation NMR experiments now can be used to resolve the microstructures of complex polymer chains. The recoupling techniques allow dipolar interactions and chemical shift anisotropy to be observed under MAS conditions, thus enabling simultaneous detection of high-resolution 1 H or 13 C signals and quasi-static anisotropic interactions. The domain sizes and interphase thickness in multiphase polymers and miscibility in polymer blends can now be determined effectively using the dipolar filter techniques. In the dynamics studies, it is now possible to obtain information on local fast motions of a single bond and super-slow chain dynamics by efficient suppression of spin-diffusion among protons and recoupling of chemical shift anisotropy. In summary, the advanced solid-state NMR techniques have enabled detailed studies on polymer microstructure, phase separation and dynamic behavior at different time and length scales, and on the relationship between the microstructure and macroscopic properties of polymers.
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Design of a Miniaturized NMR Spectrometer Console Based on FPGA
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XIAO Ying, ZHENG Zhen-Yao, CAI Shu-Hui, CHEN Zhong
Chinese Journal of Magnetic Resonance, 2012, 29(3): 346-353.
To meet the functionality requirements and the trend of instrument miniaturization, a miniaturized NMR spectrometer console system based on fieldprogrammable gate array (FPGA) and advanced RISC machines (ARM) is proposed. This digital console has the advantages of extremely high processing speed, accurate control, short development cycle and low costs. In this paper, we introduce the functions of FPGA in the system, including data receiving, parameter configuration, pulse emission and data sampling modules. The ARM embedded module achieves the function of Ethernet communication between the console and host computer, such that the internal operation of the console will not be disturbed by the network status.
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High-Resolution Diffusion-Weighted Imaging on Small Animals on a Clinical 3 T MRI Scanner
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WANG Qian-Feng, LI Jian-Qi, WU Dong-Mei, WANG Xiao-Lou, JIA Jie, ZHANG Min, LI Geng-Ying
Chinese Journal of Magnetic Resonance, 2012, 29(3): 372-378.
The most commonly used pulse sequence for small animal diffusion-weighted imaging on clinical MRI scanners is the single shot echo planar imaging (EPI) sequence. However, EPI is susceptible to off-resonance artifacts arising from the inhomogeneity of main field, local susceptibility gradients, and chemical shift, leading to image quality degradation. In this study, we implemented a high-resolution spinecho diffusion weighted imaging (SE-DWI) on a clinical 3 T MRI scanner. To reduce the motion artifacts, navigator echoes were acquired to correct the phase errors. The results from ischemic rat brain demonstrated that SE-DWI was feasible for imaging small animals on 3 T clinical MRI scanners.
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Effects of Yinao Jieyu Recipe in Intervening Cerebral Metabolism in Depressive-Like Rats Studied by In Vivo Magnetic Resonance Spectroscopy
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HUANG Yu-Ling, TANG Qi-Sheng, LI Ning, ZHU Chen-Jun
Chinese Journal of Magnetic Resonance, 2012, 29(3): 379-387.
This study investigated the metabolic change in brain of depression-like rats and the intervention effects of Yinao Jieyu recipe. Twenty rats were randomly allocated into normal group, depression group, fluoxetine group and Yinao Jieyu recipe group, with five rats in each group. The animals in the normal group were raised regularly. The animals in the other three groups were subjected to chronic unpredictable mild stress (CUMS) for 21 days. After the CUMS treatment, the animals in the depression group received saline treatment by gastrogavage for 6 weeks, and those in the fluoxetine group and Yinao Jieyu recipe group received fluoxetine and Jieyu recipe treatments, respectively, by gastrogavage for 6 weeks. In vivo 1 H MRS was performed to measure the changes of N-acetyl aspartate (NAA), choline (Cho) and creatine (Cr) levels in the left prefrontal cortex and hippocampus. Compared to the normal group, the depression group and the fluoxetine group showed significantly decreased NAA/Cr ratio in the hippocampus and frontal cortex. The Yinao Jieyu recipe group showed significantly higher NAA/Cr ratio in the hippocampus and prefrontal cortex relative to the depression group. The hippocampal Cho/Cr ratio in the depression group was found increased (P <0.05), while that in the Yinao Jieyu recipe group decreased (P <0.01), compared to the normal group. The prefrontal Cho/Cr ration in the depression group and fluoxetine group showed significant increases relative to the normal. The prefrontal Cho/Cr ratios in the Yinao Jieyu recipe group and fluoxetine group were significantly lower than that in the depression group. In conclusion, the Yinao Jieyu recipe appeared to have apparent anti-depression effects in rats subjected to CUMS.
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An Improved Detection Algorithm for Detection of Weak NQR Signals
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ZHU Kai-Ran, Wu Hui-Yang, ZHENG Ji-Bin, SU Tao
Chinese Journal of Magnetic Resonance, 2012, 29(3): 393-400.
Nuclear quadrupole resonance (NQR) is a solid-state radio frequency (RF) spectroscopic technique allowing the detection of many high explosives. However, the NQR signals are intrinsically weak, and the practical use of NQR is hindered by low signal-to-noise ratio (SNR ), and artifacts arising from the thermal noise of the coil and external radio frequency interference (RFI). In this paper, we described an improved detection algorithm for detection of weak NQR signals. First, singular value decomposition using the Hankel matrix was utilized to restrain RFI and filter noise. A non-linear least squares detector based on the (multiple signal classification) MUSIC spectral estimation was applied, which not only guaranteed a high resolution in the frequency domain, but also led to significant reduction in the amount of computation. The effectiveness of this algorithm was demonstrated with the simulated and experimental results.
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Identification and Determination of Condiritul in Xiaoaiping Injection by Nuclear Magnetic Resonance Spectrometry
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GAO Xiang, CHEN Dong-Jun, MA Yan-Chun, ZHU Dan-Ni, YU Bo-Yang
Chinese Journal of Magnetic Resonance, 2012, 29(3): 410-418.
In order to establish a quality control method for Xiaoaiping Injection, one-dimensional and two-dimensional NMR techniques used to measure the important chemical constituents, including condiritul, in the injection. An NMR method for quantitative analysis of condiritul using hydroquinone as the internal standard was presented. The proton signals of condiritul at δ 5.73 and those of hydroquinone at δ 6.73 were used for quantification. Linear regression of quantitative peak area ratio (Ax /As , y ) of condiritul-hydroquinone versus mass ratio (Wx /Ws , x ) yielded a regression equation of y =0.034 1 x +0.090 6 with a correlation coefficient of 0.999 6. The precision relative standard deviation (RSD ) was 1.27%, the reproducibility RSD 2.16% and the stability RSD 0.13%. The results showed that 1 H NMR can be used for quantitative measurement of condiritul in Xiaoaiping Injection.