高电离态Ti原子EUV光谱的实验研究

在中国原子能研究院HI-13串列加速器上用束-箔技术完成了80 MeV Ti离子和C箔相互作用产生的高电离态离子谱观测,与用激光等离子体技术的实验结果做了比较，大多数谱线与激光等离子体技术的实验结果有较好的符合，有3条谱线是未观测到的.这几条谱线为ⅩⅧ 13.406，ⅩⅧ 14.987，17.439nm, 属于2s2p^{2 4}P_3/2—2p^{3 2}D_3/2, 2s2p^{2 1}S₀—2sp^{3 1}P₁, 4p ¹P₀—5d ¹P₁跃迁. 关键词： 串列加速器 高电荷态原子 激发光谱     

HR/MAS高分辨魔角微量探头用于天然橡胶固体1H、13C NMR测试及其与液体BBO探头、固体CP/MAS探头测试的比较

采用BRUKER高分辨魔角微量探头（HR/MAS），液相宽带BBO探头和固体CP/MAS探头，对天然橡胶固体、乳液以及天然橡胶溶于氘代苯的溶液进行了¹H、¹³C 1D和2D NMR谱的测试和比较. 发现HR/MAS探头用于天然橡胶固体和乳液时可以得到高分辨的¹H、¹³C谱，克服了CP/MAS探头测试固体¹³C NMR谱或者是固体¹H NMR谱时，谱图存在S/N值可能较小、谱峰可能宽化的弱点.     

1-[2-(2,4-二氯苯基)-4-烷基-1,3-二氧戊环-2-基甲基]-1H-1,2,4-三唑的NMR研究

测定了戊环唑（1）、甲环唑（2）、丙环唑（3）的NMR谱,对其一般特征进行 了对比与讨论,用¹³C-¹H COSY、¹³C-¹H COLOC、DQF-COSY、DEPT等技术对它们的¹H、¹³C NMR谱峰进行了全归属,并应用¹H-¹H NOESY谱研究其立体结构.
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头孢菌素类化合物的核磁共振谱研究

应用¹H NMR、¹³C NMR和DEPT135°技术以及¹H-¹H COSY、HMBC、HMQC二维核磁共振技术，对头孢菌素类抗生素头孢替坦二钠、头孢曲松钠及头孢噻肟钠的质子信号和碳信号进行了全归属，并指出其核磁共振谱特征.     

南海海绵Dysidea fragilis中两个倍半萜内酯的NMR研究

用一维¹H、¹³C NMR谱、DEPT ¹³C NMR谱、选择性远程DEPT ¹³C NMR、¹H-¹H COSY和¹³C-¹H COSY二维核磁共振技术研究了南海海绵Dysidea fragilis中的两个倍半萜herbadysidolide(1)和furodysinin lactone(2),确认了化学结构,并对其¹³C NMR和¹H NMR谱进行了归属.药理活性试验表明:1和2具有一定的心血管活性.     

8,2'-O-环化-9β-D-腺嘌呤阿拉伯糖苷的NMR及结构研究

8,2'-O-环化-9β-D-腺呤阿拉伯糖苷是阿糖腺苷合成过程中的一个关键性中间体,该化合物的NMR数据只有¹H-NMR谱的糖环1'位质子化学位移和偶合常数的报道,¹³C-NMR谱未曾报道。本文用2D-NMR、NOE-DIF等技术,对它的¹H、¹³C-NMR谱进行归属,进一步明确了它的结构。     

西洋参皂甙的核磁共振波谱研究Ⅰ.西洋参叶中Ocotillol型皂甙的结构分析

本文用常规一维¹H、¹³C核磁共振波谱和远程异核化学位移相关谱。异核化学位移相关谱和同核化学位移相关谱技术研究了西洋参叶中首次分离出的一种Ocotillol型皂甙,确认了化学结构,并对其¹³C、¹H NMR谱线进行了归属。     

阿扑西林结构确证的谱学研究

对青霉素类抗生素阿扑西林的红外光谱（IR）、紫外光谱（UV）、核磁共振氢谱（¹H NMR）、氢氢相关谱（¹H-¹H COSY）、核磁共振碳谱（¹³C NMR）、DEPT谱、碳氢相关谱（HSQC）、质谱（MS）进行了解析,对其所有的NMR谱信号进行了归属,同时讨论了质谱的主要碎片离子的可能的裂解方式和红外特征吸收峰所对应的官能团的振动形式. 通过多种波谱技术确证了阿扑西林的结构.     

碘分子单频及双频多光子光谱

采用多光子离化谱和荧光激发谱技术，对碘分子单频和双频五光子离化谱和三光子荧光谱进行了研究和标识．对OODR五光子离化谱中一组间隔为72cm^-1的振动序列进行了归属，并确定了其激发、发射和离化通道 关键词：     

克林霉素磷酸酯的波谱学研究

克林霉素磷酸酯是临床上广泛使用的一种抗菌类药物. 本文对克林霉素磷酸酯进行了¹H、¹³C、³¹P NMR检测,通过DEPT、¹H-¹H COSY、¹³C-¹H HSQC、¹³C-¹H HMBC等2D NMR技术对该化合物的¹H、¹³C谱的信号进行了全归属,并结合量子化学计算和NOESY谱证实了化合物的立体结构. 另外,对克林霉素磷酸酯的飞行时间质谱(TOF-MS)的裂解途径进行了分析.     

哌嗪雌酚酮的结构研究

哌嗪雌酚酮是一种可望用于骨质疏松症的雌激素类防治药物. 文中采用IR、MS、NMR 等波谱技术,特别是¹H-1H COSY、HMQC和HMBC谱等2D NMR技术, 确定了它的氢谱和碳谱的信号归属,对它的结构进行了确证.     

Osteoporosis detection in postmenopausal women using axial transmission multi-frequency bone ultrasonometer: Clinical findings

The objective of this study was to evaluate if the Bone UltraSonic Scanner (BUSS) can detect osteoporosis in postmenopausal women. BUSS is an axial transmission multi-frequency ultrasonometer for acquisition of wave propagation profiles along the proximal anterior tibia. We derived 10 diagnostically significant BUSS parameters that were then compared with the DXA spine T-score, which was used in this study as the “gold standard” for the assessment of osteoporosis (T-score <−2.5). BUSS wave parameters were studied in 331 postmenopausal women examined by 9 trained operators at 3 clinical sites with use of 3 devices. The efficiency of each BUSS parameter in osteoporosis detection was assessed using a receiver operating characteristic curve analysis. Area under the curve (AUC) for each of 10 parameters ranged from 58.1% to 70.2%. Using these parameters a linear classifier was derived which provided at its output 83.0% AUC, 87.7% sensitivity and 63.2% specificity to DXA-identified osteoporosis. The results of this study confirm BUSS’s capability to detect osteoporosis in postmenopausal women.     

吲哚衍生物的1H NMR谱研究

通过对¹H-¹H COSY谱的分析, 鉴定了两个同分异构体吲哚衍生物取代基团的位置，并对其氢谱进行了分析，对其谱峰进行了归属. 比较了一系列吲哚衍生物类似物的的氢谱，发现其氢谱呈现一定规律，并分析了其原因.     

Design of small volume HX and triple-resonance probes for improved limits of detection in protein NMR experiments

Three- and four-frequency nuclear magnetic-resonance probes have been designed for the study of small amounts of protein. Both "HX" (1H, X, and 2H channels) and "triple-resonance" (1H, 15N, 13C, and 2H) probes were implemented using a single transmit/receive coil and multiple-frequency impedance matching circuits. The coil used was a six-turn solenoid with an observe volume of 15 microl. A variable pitch design was used to improve the B1 homogeneity of the coil. Two-dimensional HSQC spectra of approximately 1mM single labeled 15N- and double labeled 15N/13C-proteins were acquired in experimental times of approximately 2h. Triple-resonance capability of the small-volume triple-resonance probe was demonstrated by acquiring three-dimensional HNCO spectra from the same protein samples. In addition to enabling very small quantities of protein to be used, the extremely short pulse widths (1H = 4, 15N = 4, and 13C = 2 micros) of this particular design result in low power decoupling and wide-bandwidth coverage, an important factor for the ever-higher operating frequencies used for protein NMR studies.     

齐墩果酸三萜配糖体2D NMR的研究

从甘肃产的猫儿屎(Decaisnea Fargesi)植物茎中分离出三个新皂甙.利用二维核磁共振(2DNMR)技术研究确定了它们的化学结构,并对其进行了¹³C和¹H的全归属.     

2D—NMR对皂皮酸—3—氧—葡萄糖醛酸^13C,^1H的完全指定—介绍HMBC和HOHAHA

HMBC是一种测定远程偶合~1H—~(13)C相关的十分灵敏的方法,特别适用于检测和甲基质子远程偶合(~2J,~3J)的碳.HOHAHA谱显示出多次Relay信息,选择适当参数可通过一次实验得到独立自旋体系中所有质子相关信息.本文用HMBC和HOHAHA实验结合同核(~1H)COSY和导核(~(13)C-~1H)COSY确认了Qwhaic acid—3—O—glucuronic acid分子中所有~(13)C和~1H的归属.     

三种测量橡胶交联密度的核磁共振方法比较

核磁共振（NMR）技术已经成为测量橡胶交联密度的一种常用技术手段．该文探讨了用于测量橡胶交联密度的三种NMR方法：¹H双量子（DQ）NMR、¹H Hahn回波和¹H CPMG回波,讨论了这些方法测量值差异的来源．在此基础上进一步研究了¹H CPMG回波方法中回波时间对测量值的影响,探讨了改善¹H CPMG回波方法的方案．     

Sensitivity-enhanced static 15N NMR of solids by 1h indirect detection

A method for enhancing the sensitivity of 15N spectra of nonspinning solids through 1H indirect detection is introduced. By sampling the 1H signals in the windows of a pulsed spin-lock sequence, high-sensitivity 1H spectra can be obtained in two-dimensional (2D) spectra whose indirect dimension yields the 15N chemical shift pattern. By sacrificing the 1H chemical shift information, sensitivity gains of 1.8 to 2.5 for the 15N spectra were achieved experimentally. A similar sensitivity enhancement was also obtained for 2D (15)N-(1)H dipolar and 15N chemical shift correlation spectroscopy, by means of a 3D 1H/15N-1H/15N correlation experiment. We demonstrate this technique, termed PRINS for proton indirectly detected nitrogen static NMR, on a crystalline model compound with long 1H T(1rho) and on a 25-kDa protein with short 1H T(1rho). This 1H indirect detection approach should be useful for enhancing the sensitivity of 15N NMR of oriented membrane peptides. It can also be used to facilitate the empirical optimization of 15N-detected experiments where the inherent sensitivity of the sample is low.     

Analysis of 1H-NMR relaxation time distributions in L1 to L6 rat lumbar vertebrae

A better knowledge of the NMR relaxation behavior of bone tissue can improve the definition of imaging protocols to detect bone diseases like osteoporosis. The six rat lumbar vertebrae, from L1 to L6, were analyzed by means of both transverse (T(2)) and longitudinal (T(1)) relaxation of (1)H nuclei at 20 MHz and 30 degrees C. Distributions of relaxation times, computed using the multiexponential inversion software uniform penalty inversion, extend over decades for both T(2) and T(1) relaxation. In all samples, the free induction decay (FID) from an inversion-recovery (IR) T(1) measurement shows an approximately Gaussian (solid-like) component, exp[-1/2(t/T(GC))2], with T(GC) approximately 12 micros (GC for Gaussian component) and a liquid-like component (LLC) with initially simple-exponential decay. Averaging and smoothing procedures are adopted to obtain the ratio alpha between GC and LLC signals and to get separate T(1) distributions for GC and LLC. Distributions of T(1) for LLC show peaks centered at 300-500 ms and shoulders going down to 10 ms, whereas distributions of T(1) for GC are single broad peaks centered at roughly 100 ms. The T(2) distributions by Carr-Purcell-Meiboom-Gill at 600 micros echo spacing are very broad and extend from 1 ms to hundreds of ms. This long echo spacing does not allow one to see a peak in the region of hundreds of micros, which is better seen by single spin-echo T(2) measurements. Results of the relaxation analysis were then compared with densitometric data. From the study, a clear picture of the intratrabecular and intertrabecular (1)H signals emerges. In particular, the GC is presumed to be due to (1)H in collagen, LLC due to all the fluids in the bone including water and fat, and the very short T(2) peak due to the intratrabecular water. Overall, indications of some trends in composition and in pore-space distributions going from L1 to L6 appeared. Published results on rat vertebrae obtained by fitting the curves by discrete two-component models for both T(2) and T(1) are consistent with our results and can be better interpreted in light of the shown distributions of relaxation times.     

南蛇藤中倍半萜生物碱的二维NMR研究

用DEPT和二维NMR技术包括:¹H-¹H COSY,¹H-¹³C COSY,NOESY,特别是¹H-¹³C COLOC对两个多酯基取代的倍半萜生物碱的化学及立体结构进行了研究,并对其¹H和¹³C NMR谱峰进行了归属。