NMR技术在前列腺素及其类似物的化学结构分析中的应用

前列腺素（PG）及其类似物的种类多且生理作用广泛,故已引起药理、临床和药物合成工作者们的注意。目前,有几种前列腺素已应用于临床。其中PGE1、PGE2和PGF2α对计划生育颇有价值。前列腺素的分子具有一个五员环和二条侧链。除PGB 以外,其他几类前列腺素的分子都含有二个以上的手征性碳原子,和一个或二个碳-碳双键。因此。

甲磺酸加替沙星的化学结构分析

建立药物甲磺酸加替沙星化学结构的确证方法。通过热分析(TA)、元素分析(EA)、紫外吸收光谱(UV)、红外吸收光谱(IR)、质谱(MS)、X-射线粉末衍射(XRD)及核磁共振(NMR)等分析手段,对甲磺酸加替沙星样品进行结构确证。证实了甲磺酸加替沙星的结构为1-环丙基-6氟-1,4-二氢-8-甲氧基-7-(3-甲基-1-哌嗪基)-4-氧-3-喹啉羧酸甲磺酸盐。该方法准确、可行,从而为甲磺酸加替沙星的生产和鉴定提供了较全面的参考依据。

分子马达五配位磷化学结构分析

The mechanisms of molecular motors are still unresolved problems. Based on our experiments on amino acids, the activated process of molecular motors was analyzed and original software using the method of penta-coordinated phosphorous structure was designed. Via the software, the hotspots from different molecular motors′ phosphorous activated area were obtained. It was found that the types of hotspots discovered with above methods were highly conserved. This founding provides new perspectives to study the intrinsic relationship of motion in molecular motors and also helps understanding the evolution of molecular motors.

合成Fe-EDDHA化学结构分析及其生物有效性研究初报

通过对合成的Fe -EDDHA与荷兰AkzoNobel化学公司产品叶绿灵的红外光谱及核磁共振氢谱图谱分析比较 ,初步确定两者主体化学结构一致。田间生物有效性试验表明 ,合成有机螯合铁肥及荷兰产叶绿灵均可显著提高花生叶绿素含量 ,改善花生铁素营养 。

基于化学结构分析头孢曲松的皮肤试验问题

头孢曲松（ceftriaxone）是广谱、长效、耐酶的半合成第三代头孢菌素类药物，临床用于多种敏感菌所致感染的治疗。2009年，头孢曲松被列入《国家基本药物目录》，成为唯一列入基本目录的第3代头孢菌素，在临床广泛使用。最新修订的注射用头孢曲松钠（罗氏芬）药品说明书增加了给药前进行皮肤试验（皮试）的规定，与国外及国内其他生产厂家的说明书不统一，在一定程度上给临床工作带来了问题和困扰。本文着重从头孢菌素类药物化学结构方面分析其引起过敏反应的原因，

湖北省异常血红蛋白的实验筛查及变异型研究

本文报道湖北省对７种民族，１０１１１８人进行了异常血红蛋白调查，结果：检出异常血红蛋白１３４个家系，其中湖北籍１０６个家系，分布于本省３８个市县；６４个家系异常血红蛋白化学结构分析，证实有１５种变异型。

The Formation of Colored Film on Stainless Steel and the Study for Surface Structure

This paper discusses the coloration process on the stainless steel and the properties of the film. The compositions, morphology and structure of colored films on stainless steel are studied by using SEM,AES,AFM,STM. The diffusion controlled mechanisms of films and calculation formula of surface electropotential difference are discussed.

增钙煤矸石的火山灰活性研究

在原样煤矸石的分析基础上,提出一种合适的增钙活化煤矸石样,并对其进行火山灰活性的测定,结果表明,在煤矸石的增钙活化过程中掺入适量的石膏和萤石等组分作为矿化剂时,能生成较多的水硬性矿物且其火山灰活性较佳;活性评定实验表明,在增钙活化煤矸石与氧化钙的复合体系中,Ca(OH)2含量和化学结合水量随龄期的变化规律与其水化过程的结构特征是一致的.

A New Cyclic Bisdesmoside from Tubers of Bolbostemma paniculatum

The structure of tubeimoside V (1), a new cyclic bisdesmoside, isolated from tubers of Bolbostemma paniculatum (Tu Bei Mu), was established by means of 2D NMR spectral and chemical methods. Compound 1 has inter-saccharide chain bridging by a dicrotalic acid to form a unique macrocyclic structure.

Behavior of phenol adsorption on thermal modified activated carbon

Adsorption process is acknowledged as an effective option for phenolic wastewater treatment. In this work, the activated carbon （AC） samples after thermal modification were prepared by using muffle furnace. The phenol ad- sorption kinetics and equilibrium measurements were carried out under static conditions at temperature ranging from 25 to 55 ~C. The test results show that the thermal modification can enhance phenol adsorption on AC samples. The porous structure and surface chemistry analyses indicate that the decay in pore morphology and decrease of total oxygen-containing functional groups are found for the thermal modified AC samples. Thus, it can be further inferred that the decrease of total oxygen-containing functional groups on the modified AC sam- ples is the main reason for the enhanced phenol adsorption capacity. For both the raw sample and the optimum modified AC sample at 900 ~C, the pseudo-second order kinetics and Langmuir models are found to fit the exper- imental data very well. The maximum phenol adsorption capacity of the optimum modified AC sample can reach 144,93 mg.g ~ which is higher than that of the raw sample, i.e. 119.53 mg.g 1. Adsorption thermodynamics analysis confirms that the phenol adsorption on the optimum modified AC sample is an exothermic process and mainly via physical adsorption.

Study of Synthesis of Copoly (lactic acid/glycolic acid) by Direct Melt Polycondensation

A two steps direct copolymerisation process was developed. The first step is to produce oligomer and then the oligomer of lactic acid/glycolic acid (90/10) is polymerized with binary catalyst tin chloride dihydrate/p-toluenesulfonic acid. In this way, the direct synthesis of copoly (lactic acid/glycolic acid) without any organic solvent was investigated. The properties and structures of products were characterized by nuclear magnetic resonance (NMR), differential scanning calorimetry (DSC), X-ray diffraction and so on. The results show that comparatively high molecular weight copolymer of lactic acid and glycolic acid can be prepared by direct processing under appropriate technological conditions.

Low Temperature One-Step Synthesis of Barium Titanate:Thermodynamic Modeling and Experimental Synthesis

A thermodynamic model has been developed to determine the reaction conditions favoring low temperature direct synthesis of barium titanate (BaTiO3). The method utilizes standard-state thermodynamic data for solid and aqueous species and a 0ebye-Huckel coefficients model to represent solution nonideality. The method has been used to generate phase stability diagrams that indicate the ranges of pH and reagent concentrations, for which various species predominate in the system at a given temperature. Also, yield diagrams have been constructed that indicate the concentration, pH and temperature conditions for which different yields of crystalline BaTiO3 can be obtained. The stability and yield diagrams have been used to predict the optimum synthesis conditions (e.g., reagent concentrations, pH and temperature). Subsequently, these predictions have been experimentally verified. As a result, phase-pure perovskite BaTiO3 has been obtained at temperature ranging from 55 to 85℃ using BaCl2, TiCl4 as a source for Ba and Ti, and NaOH as a precipitator.

Theoretical Study of the AIEt3-Promoted Tandem Reductive Rearrangement of Epoxides

The AIEt3-promoted tandem reductive rearrangement reactions of epoxides was studied at B3LYP/6- 31C（d,p） level. For the model compound α-hydroxy epoxides, two possible reaction pathways Ⅰ and Ⅱ were calculated. The main difference is the order of ethylene release and six- to five-member ring rearrangement. The ring contraction rearrangement in pathway Ⅰ is the first step and this step is the rate controlling step with a free energy barrier of 116.62 kJ/mol. For pathway Ⅱ, the ethylene release occurs first, and is followed by a six-member ring opening reaction which is the rate controlling step, and the barrier is 251.38 kJ/mol. The reason for such high barrier is that the ethylene release results in the following reaction being more difficult. The results show that pathway Ⅰ （C-C rearrangement and then ethylene release） is more favorable, which is consistent with experimental results.

Translocation of Polymer Chains Through a Channel with Complex Geometries

The elastic behavior of a single chain transporting through complex channel which can be seen as the combination of three different channels （left channel, middle channel, and right channel, respectively） is investigated using the new pruned-enriched Rosenbluth method with importance sampling. The elastic force during the translocation process is calculated. At the entrance into the middle channel, there is the first plateau in the curve of the elastic force f （f〉0） versus x, here x represents the position of the first monomer along the x-axis direction. When the first monomer moves to a certain position, a second plateau is observed with the elastic force f〈0, which represents spontaneous translocation. The free energy difference between the subchain in the right channel and the subchain in the left channel may drive the transloeation. The influence of chain length and width of the left and right channels on the translocation process are also investigated. From the simulation results, more detailed explanations for the reason why the component translocation time is not the same for different channels can be presented.

Microstructure Analysis for Chemical Interaction between Cesium and SUS316 Steel in Fast Breeder Reactor Application

The objective of this study is to presume cesium corrosion process and its dominant factors in SUS316 steel, a fuel cladding material for fast breeder reactor application, based on both experimental results of cesium corrosion out-pile test and thermodynamic consideration. The cesium corrosion test was performed in simulated environment of high burn-up fuel pin. And main corrosion products in the specimen after the corrosion test were specified by TEM （transition electron microscopy） and SEM （scanning electron microscopy） in order to formulate a hypothesis of the cesium corrosion process. At the end of this study, it was found that the dominant factors of the corrosion process are the amount of cesium on the surface of the specimen, chromium content in the alloy, the supply rate of oxygen and temperature.

Intergranular Corrosion of UNS S31803 Heat Treated at 800 ℃ Varying Range Times

The aim of this work is evaluate the intergranular corrosion on UNS S31803 steel, with heat treatments at 800 ℃, varying treatment times of 30 mins, 360 mins and 1,440 mins. The results confirm the formation of o phases and secondary austenite （γ2）. For the analysis of the influence of o and γ2 phases, metallographic analysis were conducted through optical microscopy, potentiokinetic reactivation electrochemical techniques and potentiodynamic polarization in NaCI 3.5% solution. Microstructural analysis has shown a formation of γ2 and o phase in heat treatment, due to diffusion of chromium and molybdenum from δ phase to y phase, precipitating on δ/γ and δ/δ interfaces. The DL-EPR （Double loop electrochemical potentiokinetic reactivation） results have shown an increase of the DOS （degree of sensitization） for long periods of time on heat treatment. The results of potentiodynamic polarization showed a reduction of the corrosion and pitting potentials, followed by an increase of the current density when the UNS S31830 steel is heat treated during long periods of time.

Formation of [3]Pseudorotaxanes from β-cyclodextrin and a Series of Dicarboxylic Acids with Their Corresponding α,ω-alkanedicarboxylate Anions

Inclusion complexes between β-cyclodextrin （β-CD） and a series of dicarboxylic acids （DAn, n=11-15） were prepared by co-grinding and co-precipitation methods and the [3]pseudorotaxane structure of them was elucidated by FTIR, DTA and XRD characterizations. Inclusion complexes of β-CD and α,ω-alkanedicarboxylate anions （DAn^2-） were acquired by neutralizing β-CD/DAn different inclusion complexes with sodium hydroxide and the structure was also proved to be a pseudorotaxane structure by ^1H-NMR spectra and NOESY spectrum. Both the inclusion complexes of β-CD/DAn and β-CD/DAn^2- adopt the [3]pseudorotaxane structure with β-CD arranged in dimers threaded onto one aliphatic chain and the binding mode of 1：1 inclusion complex was excluded based on the consideration of chain conformations.

One-pot synthesis and structural characterization of urea-isobutyraldehyde-formaldehyde resin

Urea-isobutyraldehyde-formaldehyde (UIF) resin was synthesized from urea, isobutyraldehyde, and formaldehyde using sulfuric acid as a catalyst by one pot method. The effects of molar ratios of isobutyraldehyde to formaldehyde (n(I)/n(F)) and aldehyde to urea (n(A)/n(U)) on the yield, hydroxyl value (vs KOH) and softening point of the resin were investigated. The structure of the resin was characterized by FT-IR, 1H-NMR and 13C-NMR. The results show that when the molar ratio of urea to isobutyraldehyde to formaldehyde (n(U)/n(I)/n(F)) is 1.0/3.0/3.0, the yield UIF resin is 67.1%, and the softening point and hydroxyl value are 88 ℃ and 37 mg/g, respectively. The FT-IR, 1H-NMR and 13C-NMR results show that the lactam is formed by aminomethylation from urea, isobutyraldehyde, and formaldehyde.

Ab initio Study on Structures and Isomerization of Magnesium Fluorosilylenoid H2SiFMgF

The structures and isomerization of magnesium fluorosilylenoid H2SiFMgF were investigated by ab initio molecular orbital theory. Four equilibrium structures and three isomeric transition states were located and fully optimized at the B3LYP/6-31G（d,p） and G3MP2B3 levels, respectively. Based on the B3LYP/6- 31G（d,p） optimized geometries, harmonic frequencies of various structures were obtained and 29Si chemical shifts were calculated. The solvent effects were investigated by means of the polarizable continuum model using THF as a solvent at B3LYP/6-31G（d,p） level. Isomerization paths for isomers were confirmed by intrinsic reaction coordinate calculations. The calculated results show that tetrahedral structure has the lowest energy and is the most stable; tetrahedral, three-membered ring, and p-complex structures are suggested to be the experimentally detectable ones; and a-complex structure has the highest energy and will not exist.