混合物中稀土元素的NMR法测定

核磁共振检测混合物中的共存金属是新近发展起来的无机分析方法。Fedorov以EDTA和NTA为配体,通过观察络合物Ln(EDTA)和Ln(NTA)_2配体的~1H NMR谱线,率先开展了水溶液中共存稀土元素的同时间接测定研究,这种方法比分别直接检测各稀土核磁核共振信号的方法实用可靠,且方便易行。但采用~1H NMR谱检测水溶液中顺磁稀土离子时,强的溶剂水峰易掩蔽近邻的稀土配合物谱线;某些重稀土配合物的~1H谱线宽,相互重叠,难以用作分

用NMR方法研究杂多酸HPA-23与谷胱甘肽的作用

早在70年代初,人们就发现杂多酸具有抗病毒活性.例如钨锑酸钠[NaSb_9W_(21)O_(86)]~(18-)有可能成为潜在的抗病毒化合物.非常有趣的是最近报道[NH_4]_(18)[NaSb_9W_(21)O_(86)]·24H_2O(结构代号为HPA-23)具有很高的抗爱滋病病毒活性,在法国已进入临床应用.但从分子水平研究杂多酸化合物抗病毒的机理,目前尚未见到国内外报道.而作为病毒可以广义地看作由一个蛋白外壳包裹,内部则为核酸.爱滋病病毒同样由两层蛋白所包裹,与宿主细胞发生吸附作用主要是通过外层包络蛋白(GP120),该蛋白的活性组分是一个由8个氨基酸组成

用NMR方法研究稀土离子对DPPC脂质体构象的影响

随着稀土元素在工农业中的广泛应用,稀土进入机体内的作用机理是人们日益关心的问题.而稀土对生物体的作用,首先是通过生物膜.因此研究稀土与生物膜的作用是阐明其生理过程的重要环节.生物膜的结构比较复杂,而磷脂脂质体却能表现出生物膜膜脂结构的许

M(EGTA)配合物的NMR研究

乙二醇-双-(α-氨基乙基醚)四乙酸(EGTA)是一种Ca~(2+)高选择性螯合剂,结合Ca~(2+)能力比Mg~(2+)强10~6倍,被认为是钙结合蛋白钙结合位的理想配位模型。Ca(EGTA)的晶体结构虽已确定,但其溶液结构仍不清楚。考虑Ca~(2+)离子半径(0.99

SEQUENCE STRUCTURE OF ETHYLENE-VINYL SUBSTITUTED COPOLYMER WITH C-13 NMR .4.

The substituent chemical shift (SCS) has been applied to the assignment of the C-13 NMR spectrum of chlorinated polyethylene (CPE). CPE of different chlorine contents has been employed and their sequence structure discussed. The results show that characteristic of CPE with medium chlorine content is the dichloroethane structure in molecular chain. SCS parameters have been obtained from the C-13 NMR spectra. It was found that the effects of chlorine content and temperature on SCS are negligible, but the substituent parameter S1 reduced by 0.39 ppm when C2Cl4 was added to solvent ODCB.

A HIGH-RESOLUTION SOLID-STATE NMR-STUDY OF THE MISCIBILITY, MORPHOLOGY, AND TOUGHENING MECHANISM OF POLYSTYRENE WITH POLY(2,6-DIMETHYL-1,4-PHENYLENE OXIDE) BLENDS

An extended Goldman-Shen pulse sequence was used to observe indirectly the proton spin diffusion in the blends of polystyrene (PS) with poly(2,6-dimethyl-1,4-phenylene oxides) (PPO). The results indicate that the average distance between PS and PPO is less than 5 angstrom in the intimately mixed phase, but there are heterogeneous domains on a 100-angstrom scale. The data of spin relaxation of carbons, T1(C), for homopolymers and their blends suggest that there is a strong pi-pi electron conjugation interaction between the aromatic rings of PS and those of PPO, while the aromatic rings of PPO drive the aromatic rings of PS to move cooperatively. It is the cooperative motion that markedly improves the impact strength of PS.

C-13 NMR CHARACTERIZATION OF SOLUBLE POLYANILINE

A high-resolution C-13 n.m.r. spectrum of soluble polyaniline in DMF-d7 solution was recorded. The assignment for the various resonance peaks in the spectrum was tentatively performed and the chain structure of polyaniline was analysed. It has been shown that the main chain of pristine state polyaniline is composed of alternating benzoid-quinoid and successive benzoid-quinoid sequences with the former being present in greater concentration. The sequence distribution is random. In addition to the benzoid-type and quinoid-type structures, there is a small amount of other structural units in the main chain.

NMR-STUDIES ON THE COORDINATION OF RARE-EARTHS WITH GLYCYL-DL-VALINE AND THE CONFORMATION OF THEIR COMPLEX IN AQUEOUS-SOLUTION

In this paper lanthanide-induced shifts have been measured for C-13 and H-1 nuclei of glycyl-DL-valine in the presence of three lanthanide cations (La3+, Ho3+ and Yb3+) in aqueous solution. The stability constants of the coordination compounds of rare earths (Ho, Yb) with glycyl-DL-valine have been calculated. The coordination of rare earths with the ligand has been discussed. The simulation for conformation of lanthanide coordination compounds with glycyl-DL-valine shows that the ligand is coordinated to lanthanide ion through oxygen atoms of carboxyl group and the bond length of Ln-O is 0.226 nm. In the coordination compounds glycyl-DL-valine is in extended state with minimal steric hindrance.

SOLID-STATE C-13 NMR-STUDIES ON THE CONDENSATION AND SULFONATION OF FURFURYL ALCOHOL AND TRIS (2-HYDROXYETHYL) ISOCYANURATE

The condensation and sulfonation of furfuryl alcohol (FA) and FA with tris (2-hydroxyethyl) isocyanurate (THEIC) and the crosslinking product structures were studied by means of solid-state C-13 NMR. The reaction of formalin with FA linear oligomer terminated by 2-methyl furan took place in the presence of the phase transfer catalyst (C4H9)4N+I-. The reaction of the terminated oligomer with a large amount of sulfuric acid as well as the former reaction was examined. The effects of some main reaction conditions on the crosslinking condensation and sulfonation were also discussed.

C-13 AND H-1 NMR STUDIES OF SOLUTION STRUCTURE OF LANTHANIDE COMPLEX WITH GLYCYL-GLYCINE

C-13 and H-1 NMR technique was used to study the interaction of Gly-Gly with heavy lanthanide cations Dy3+, Ho3+, Er3+, Tm3+ and Yb3+ in aqueous solution. The stability constants for the 1:1 and 1:2 complexes of Gly-Gly with Ho3+ and Yb3+ were determined from the titration curves of chemical shift versus concentration ratio of lanthanide to Gly-Gly. The solution structure of the Ln-Gly-Gly complex was analyzed based upon the C-13 and H-1 lanthanide induced shifts and the results show that in the complex Gly Gly is coordinated to the lanthanide ion through the carboxyl oxygens with the backbone of the ligand in an extended state.

用NMR方法研究稀土离子对DPPC脂质体极性基团构象的影响

稀土对生物体的作用首先是通过生物膜,因此研究稀土与生物膜的作用是阐明其生理过程的重要环节.~2H四极劈裂和稀土位移试剂两种方法的研究结果表明,二棕榈酸磷酯酰胆碱(DPPC)的极性基团在金属离子的作用下,由原来的平行于膜平

环氧乙烷--四氢呋喃无规共聚醚结构研究 Ⅰ．液体共聚醚链结构的NMR分析

环氧乙烷(EO)与四氢呋喃(TO)的端羟基液体共聚醚(ETO),其流动性好,粘结性强,易固化,燃烧完全以及热稳定性较好,是固体推进剂的优质粘合剂。本工作对M_n为2000～6000不同组份的ETO,制备30%(V/V)的CDC13溶液,用Unity—400 NMR谱仪,定量测定了ETO链结构各组成参数及其序列分布。

聚甲基丙烯酸乙酯链结构的NMR研究

聚甲基丙烯酸乙酯(PEMA)是聚甲基丙烯酸甲酯(PMMA)的同系物.它的链结构和NMR波谱一直为人们所关注.图1是PEMA的~(13)C谱.图中溶剂峰除外,聚合物六个碳的谱峰分在三处.低场一组峰是羧基

用NMR方法研究山莨菪碱与DPPC脂质体的相互作用

山莨菪碱能够改善微循环,对治疗中毒性休克有明显疗效,已在临床上广泛应用。该药与生物膜相互作用的研究是阐明其分子药理的关键。本工作以DPPC脂质体为生物膜模型,用NMR方法研究了与山莨菪碱的相互作用。

水溶液中稀土离子与甘氨酰丙氨酸作用的NMR研究

利用~1H和~(13)C NMR技术研究了水溶液中稀土离子与二肽甘氨酰丙氨酸(以下简称甘-丙二肽,记为GA)的配位作用。由稀土诱导位移的浓度依赖关系计算了Yb与甘-丙二肽配合物的稳定常数。测定了重稀土离子Dy~(3+)、Ho~(3+)、Er~(3+)、Tr~(3+)和Yb~(3+)作用下GA的~(13)C诱导位移,并根据Reuben方法对稀土诱导位移进行了线性相关分析。对配合物中配体骨架构象的模拟分析指出,Cl-C_2-N-C_3为旁式,C_2-N-C_3-C_4和C_5-C_2-N-C_3为反交叉式。系统比较了4种含甘氨酰二肽的侧基大小对配合物稳定常数、配体构象和配合物溶液结构的影响。