医药-护肤品中氯霉素和1,2-丙二醇的分析方法

医药－护肤品中氯霉素和１，２－丙二醇的分析方法是先进行氯霉素和１，２－丙二醇的富集，再用高效液相色谱、元素分析、质谱分析、红外光谱分析、无机金属离子测定对氯霉素富集物定性分析，用高效液相色谱分析、红外光谱分析、无机金属离子测定对１，２－丙二醇富集物定性分析，色谱外标法完成氯霉素和１，２－丙二醇的定量分析。本发明解决了未知成分的被浓缩富集问题，对被检测的物品可定性、定量分析，应用领域的广泛性。

Crystallization and phase behavior of crystalline syndiotactic 1,2-polybutadiene/isotactic polypropylene blends in solution-cast thin films

Crystallization and phase behavior in solution-cast thin films of crystalline syndiotactic 1,2-polybutadiene (s-1,2-PB) and isotactic polypropylene (i-PP) blends have been investigated by transmission electron microscopy (TEM), atomic force microscopy (AFM) and field-emission scanning electron microscopy (FESEM) techniques. Thin films of pure s-1,2-PB consist of parallel lamellae with the c-axis perpendicular to the film plane and the lateral scale in micrometer size, while those of i-PP are composed of cross-hatched and single-crystal-like lamellae. For the blends, TEM and AFM observations show that with addition of i-PP, the s-1,2-PB long lamellae become bended and i-PP itself tends to form dispersed convex regions oil a continuous s-1,2-PB phase even when i-PP is the predominant component, which indicates a strong phase separation between the two polymers during film formation. FESEM micrographs of both lower and upper surfaces of the films reveal that the s-1,2-PB lamellae pass through i-PPconvex regions from the bottom, i.e. the dispersed i-PP regions lie on the continuous s-1,2-PB phase. The structural development is attributed to an interplay of crystallization and phase separation of the blends in the film forming process.

Syntheses, structures and near-IR luminescent studies on ternary lanthanide (Er-III, Ho-III, Yb-III, Nd-III) complexes containing 4,4,5,5,6,6,6-heptafluoro-1-(2-thienyl)hexane-1,3-dionate

The ligand Hhfth [4,4,5,5,6,6,6-heptafluoro-1-(2-thienyl)hexane-1,3-dione], which contains a heptafluoropropyl group, has been used to synthesize several new ternary lanthanide complexes (Ln = Er, Ho, Yb, Nd) in which the synergistic ligand is 1,10-phenanthroline (phen) or 2,2'-bipyridine (bipy). The two series of complexes are [Ln(hfth)(3)phen] [abbreviated as (Ln)1, where Ln = Er, Ho, Yb] and [Ln(hfth)(3)bipy] [abbreviated as (Ln)2, where Ln = Er, Ho, Yb, Nd]. Members of the two series have been structurally characterized. The growth morphology, diffuse reflectance (DR) spectra, thermogravimetric analyses, and photophysical studies of these complexes are described in detail. After ligand-mediated excitation of the complexes, they all show the characteristic near-infrared (NIR) luminescence of the corresponding Ln(3+) ions (Ln = Er, Ho, Yb, Nd). This is attributed to efficient energy transfer from the ligands to the central Ln(3+) ions, i.e. an antenna effect. The heptafluorinated substituent in the main hfth sensitizer serves to reduce the degree of vibrational quenching. With these NIR-luminescent lanthanide complexes, the luminescent spectral region from 1300 to 1600 nm, which is of particular interest for telecommunication applications, can be covered completely.

Fe(2-EHA)(3)/Al(i-Bu)(3)/hydrogen phosphite catalyst for preparing syndiotactic 1,2-polybutadiene

Polymerizing 1,3-butadiene into syndiotactic 1,2-polybutadiene with art iron(III) catalyst system has been investigated. Activity of the catalyst was affected by the type of cocatalyst alkylaluminum and the phosphorus compound as an electron donor, molar ratio of catalyst components, and their aging sequence and aging time of the catalyst. The microstructure and configuration of the polymer was decided by the catalyst components, the higher [Al]/[Fe] molar ratio tending to yield syndiotactic 1,2-polybutadiene, while the higher [P]/[Fe] molar ratio favors the formation of amorphous 1,2-polybutadiene.

Poly[di-mu(3)-chloro-mu(2)-trans-1,2-di-4-pyridylethylene-dicopper(I)]: a two-dimensional organic-inorganic hybrid constructed from linear CuCl clusters and bridging ligands

The structure of the title compound, [Cu2Cl2(C12H10N2)](n), contains infinite CuCl staircase-like chains, which lie about inversion centres. The trans-1,2-di-4-pyrid-ylethyl-ene mol-ecules also lie about inversion centres and connect the CuCl chains through Cu-N coordination bonds into a two-dimensional organic-inorganic hybrid network. The planar sheets are stacked along the c axis and associated through weak C-H center dot center dot center dot Cl inter-actions. The results show a reliable structural motif with controllable separation of the CuCl chains by variation of the length of the ligand.

catena-Poly[[[2-(2-furyl)-1H-imidazo[4,5-f][1,10]phenanthroline]zinc(II)]-mu-benzene-1,2-dicarboxylato]

In the title compound, [Zn(C8H4O4)(C17H10N4O)](n), the Zn-II atom is five-coordinated by two N atoms from the phenanthro-line-derived ligand and three O atoms from one bidentate and one monodentate benzene-1,2-dicarboxylate (1,2-BDC) dianions in a distorted trigonal-bipyramidal geometry. The Zn-II atoms are bridged by the 1,2-BDC ligands to form a single-chain structure. Neighboring chains interact through pi-pi interactions, leading to a two-dimensional network.

用核磁共振方法表征6(8)氨基-3H苯[1,2]氧嗪-1,4-二酮

用一维1HNMR、13CNMR方法研究了6(8)氨基-3H苯[1,2]氧嗪-1,4二-酮的结构,并通过二维1H-1H同核相关谱(COSY)、13C-1H异核相关谱(HMQC)及13C-1H异核远程相关谱(HMBC)进一步确定了该类化合物的1H谱和13C谱中各谱峰的归属,为研究同类化合物表征提供了依据。

填充油的种类对Fe系1,2-聚丁二烯性能的影响

研究了芳烃油和环烷烃油对充油铁系1,2-聚丁二烯橡胶性能的影响。结果表明,基础胶充油后门尼粘度值下降,可塑性增加,混炼行为变佳;填充芳烃油比填充环烷烃油的橡胶在拉伸强度、撕裂强度、伸长率和生胶门尼值等方面均有所提高;充油后虽然硫化胶硬度降低,但是生热和耐磨性能提高。填充芳烃油可适当提高硫化胶的抗湿滑性,但滚动阻力也升高。环烷烃油可降低硫化胶的滚动阻力。充油可适当改善胶料的抗老化性能。

间同立构1,2-聚丁二烯的合成和形态结构研究

间同立构1,2-聚丁二烯自1955年问世以来 ,引起人们的广泛关注 ,但绝大多数研究工作集中在聚合物的合成方面[1～3] ,对其形态结构方面的研究却很少报道[4] ,原因是该聚合物分子侧链含有大量双链 ,在较高温度下 (>150℃ )很容易产生热交联 ,这给结构研究造成了很大困难 .间同立构1,2-聚丁二烯的性能取决于间规度 ,低间规度聚合物呈现弹性体特征 ,而高间规度聚合物则是一种半结晶性塑料 ,其结晶为平面锯齿链正交堆砌 ,Pacm空间群[4] .本文采用一种新的催化体系 ,使合成的1,2-聚丁二烯间规度可以调控.同时首次报道了结晶性间规1,2-聚丁二烯稀溶液浇铸薄膜形成具有单晶取向的板条状片层结构,并应用电子显微学和电子衍射技术确定其晶体结构.1.实验部分1.1样品及试剂　乙酰基丙酮铁 [(Fe(acac) 3)纯度为 99.9% ],使用时配成0.2mol/ L的甲苯溶液 ;三异丁基铝 [Al(i-Bu) 3]由 Aldrich公司提供 ;氢化亚磷酸二乙酯 (DEP)及丁二烯由锦州化学公司提供 ;丁二烯通过蒸馏进行纯化 ;己烷使用前在 Na/ K合金...

结晶性间同立构1,2-聚丁二烯的单晶结构

近十几年来,结晶性间同立构1,2-聚丁二烯引起人们的广泛关注,但绝大多数研究工作集中在聚合物的制备、物理性质和应用方面[1～3],对于其结晶行为和晶体结构则未见报道 .原因是间同立构1,2-聚丁二烯分子侧链含有大量的双键,在较高温度下很容易交联 ,特别是高间规度的聚合物 ,由于其熔融温度高 (>200℃ )则更易产生交联,这给结晶行为和结构研究带来很大困难.结晶性间同立构1,2-聚丁二烯的晶体结构为平面锯齿链正交堆砌,Pacm空间群[4].我们曾报道了结晶性间同立构1,2-聚丁二烯的合成和溶液浇铸膜的板条状结构[5],本文采用薄膜熔体结晶的方法第一次成功地获得了间同立构1,2-聚丁二烯的单晶,并通过电子显微学和电子衍射技术确定了其晶体结构.1 实验部分1.1间同立构1,2-聚丁二烯的制备采用乙酰基丙酮铁 [Fe(acac) ]3、三异丁基铝 [Al(i-Bu)3]和氢化亚磷酸二乙酯 (DEP)的新催化体系制备间同立构1,2-聚丁二烯,具体合成路线参见文献 [5].本文所选用聚合物的1,2单元含量为 89.3 % ,间规度为 ...

Preparation, characterization and quantized capacitance of 3-mercapto-1,2-propanediol monolayer protected gold nanoparticles

Monolayer protected gold nanoparticles (MPCs) are the focus of recent research for their stability and are deemed as the building blocks of bottom-up strategies. In this Letter, 3-mercapto-1,2-propanediol monolayer protected gold nanoparticles (MPD-MPCs) were synthesized and characterized by transmission electron microscopy, UV/Vis spectroscopy, X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy. The value of quantized double-layer capacitance (1.13 aF) of MPD-MPCs in aqueous media was obtained by differential pulse voltammograms.

Systematic study of the transfer of amino acids across the water/1,2-dichloroethane interface facilitated by dibenzo-18-crown-6

Facilitated ion transfer reactions of 20 amino acids with di.benzo-18-crown-6 (DB18C6) at the water/1,2-dichloroethane (W/DCE) interfaces supported at the tips of micro- and nano-pipets were investigated systematically using cyclic voltammetry. It was found that there were only 10 amino acids, that is, Leu, Val, Ile, Phe, Trp, Met, Ala, Gly, Cys, Gln (in brief), whose protonated forms as cations can give well-defined facilitated ion transfer voltammograms within the potential window, and the reaction pathway was proven to be consistent with the transfer by interfacial complexation/dissociation (TIC/TID) mechanisms. The association constants of DB 18C6 with different amino acids in the DCE (beta(0)), and the kinetic parameters of reaction were evaluated based on the steady-state voltammetry of micro- or nano-pipets, respectively The experimental results demonstrated that the selectivity of complexation of protonated amino acid by DB18C6 compared with that of alkali metal cations was low, which can be attributed to the vicinal effect arising from steric hindrance introduced by their side group and the steric bulk effect by lipophilic stabilization.

Studies of effect of phase volume ratio on transfer of ionizable species across the water/1,2-dichloroethane interface by a three-electrode setup

The electrochemical behavior of pyridine distribution at the water/1,2-dichloroethane interface with variable phase volume ratios (r=V-0/V-W) was investigated by cyclic voltammetry. The system was composed of an aqueous droplet supported on a Ag/AgCl disk electrode covered with an organic solution or an organic droplet supported on a Ag/AgTPBCl disk electrode covered with an aqueous solution. In this way, a conventional three-electrode potentiostat can be used to study an ionizable compound transfer process at a liquid/liquid interface with a wide range of phase volume ratios (from 0.0004 to 1 and from 1 to 2500). Using this special cell we designed, only very small volumes of both phase were needed for r equal to unity, which is very useful for the investigation of the distribution of ionizable species at a biphasic system when the available amount of species is limited. The ionic partition diagrams were obtained for different phase volume ratios.

Electrochemical recognition of alkali metal ions at the micro-water 1,2-dichloroethane interface using a calix[4]arene derivative

In this paper, a calix[4]arene derivative, 5,11,17,23-butyl-25,26,27,28-tetra-(ethanoxycarbonyl)-methoxy-calix[4]arene (L), is investigated as a host to recognize alkali metal ions (Li+, Na+, K+, Rb+ and Cs+) at the interface between two immiscible electrolyte solutions (ITIES). Well-defined cyclic voltammograms are obtained at the micro- and nano-water \ 1,2-dichloroethane (W \ DCE) interfaces supported at micro- and nano-pipets.

Study of ionizable drugs transfer across the water/1,2-dichloroethane interface with phase volume ratio equal to unity using a three-electrode system

The electrochemical behavior of ionizable drugs (Amitriptyline, Diphenhydramine and Trihexyphenedyl) at the water/1,2-dichloroethane interface with the phase volume ratio (r = V-o/V-w) equal to 1 are investigated by cyclic voltammetry. The system is composed of an aqueous droplet supported at an Ag/AgCl disk electrode and it was covered with an organic solution. In this manner, a conventional three-electrode potentiostat can be used to study the ionizable drugs transfer process at a liquid/liquid interface. Physicochemical parameters such as the formal transfer potential, the Gibbs energy of transfer and the standard partition coefficients of the ionized forms of these drugs can be evaluated from cyclic voltammograms obtained. The obtained results have been summarized in ionic partition diagrams, which are a useful tool for predicting and interpreting the transfer mechanisms of ionizable drugs at the liquid/liquid interfaces and biological membranes.