Separation and determination of active components in Radix Salviae miltiorrhizae and its medicinal preparations by nonaqueous capillary electrophoresis

A nonaqueous capillary electrophoresis (NACE) method was developed for simultaneous assay of three bioactive components (1: cryptotanshinone; 2: tanshinone IIA, and 3: tanshinone I) in Radix Salviae miltiorrhizae and in its herbal preparations for the first time. After optimization of separation conditions, a buffer of 250 mmol L(-1) ammonium acetate containing 30% acetonitrile and 1.0% acetic acid (V:V) in methanol was selected for separating the three analytes, but baseline separation of tanshinon I and tanshinone IIA was not obtained. Therefore second-order derivative electropherograms were applied for resolving overlapping peaks. Regression equations revealed good linear relationships (correlation coefficients 0.9943-0.9991) between peak heights in second-order derivative electropherograms and concentrations of the three analytes. The relative standard deviations (RSD) of the migration times and the peak height of the three constituents were in the range of 0.81 -0.88% and 0.34-1.13% (intra-day), 1.57-1.86% and 3.05-5.52% (inter-day), respectively. The recoveries of three constituents ranged from 90.2 to 108.5%. The results indicated that baseline separation of the analytes was sometimes hard to obtain and second-order derivative electropherograms were applicable for the resolving and analysis of overlapping peaks.     

PW1700X射线衍射仪织构分析应用软件的功能开发

由Ｐｈｉｌｉｐｓ引进的ＰＷ１７００Ｘ射线衍射仪织构测量系统只能用反射法，按螺旋线扫测极目数据，测绘极角。α≤８５°的不完整极图。经功能开发后，建立了织构分析测算系统，织构分析应用软件包，包括不完整极图测量与ＯＤＦ（取向分布函数）计算，回算全极图与反极图，可彩色屏显考贝，并能进行织构的定量分析。适用于立方和六方品系多晶织构材料分析。近两年应用表明，软件功能优异。     

毛细管电色谱柱内径对电渗流与电压关系的影响

考察不同内径的毛细管电色谱柱中分离电压对电渗流的影响，在不同内径的毛细管电色谱柱中，电渗流与电压都呈较好的线性关系，与毛细管电色谱柱的内径无关，由于焦耳热的影响，在电压变化幅度较大的情况下，电渗流与电压的关系曲线呈线性弯曲，在大内径毛细管电色谱柱上更加明显。     

The study of the emulsification efficiency of Aerosil and HPMCAS type and their ratio to stabilize emulsions of zedoary turmeric oil

The solid particles or polymers were often solely used to stabilizing emulsions, as an interesting alternative to classical used emulsifiers. However, a united use of them and the relation between them at stabilizing emulsions were little reported. Our previous study showed that the preparation of microspheres containing zedoary turmeric oil (ZTO, as an oily drug), Aerosil200 particles and hydroxypropyl methylcellulose acetate succinate (HPMCAS). ZTO emulsions were produced when the microspheres were immersed into aqueous media and disaggregated under gentle agitation, and were stabilized by Aerosil200 particles and HPMCAS. Nevertheless, more work needs to be carried out to explain the factor affecting emulsification efficiency of microspheres, which will facilitate the design of the microsphere formulation. Thus, in this study, we dealt with a system consisting of Aerosil, HPMCAS, ZTO and water. To predict the best ratio of Aerosil/polymer and thus obtain the best satisfying ZTO emulsions, the bonding studies were carried out with Aerosil and HPMCAS. A series of emulsions was prepared and the stability and droplet size of resultant emulsions were investigated. The results indicated two kinds of HPMCAS (HPMCAS-LG and -HG) showed the different affinity for Aerosil200, which resulted in the unlike capability to stabilize emulsions when at the same Aerosil/polymer ratio. The stability and droplet size of emulsions increased on increasing the ratio Aerosil to polymer, and the best ratio was predictable from the Langumuir-fit of the adsorption isotherms. Appropriate hydrophilicity and hydrophobicity with Aerosil particles were very important to stabilizing the ZTO emulsions.     

On the enantioselective hydrogenation of isomeric β-acylamido β-alkylacrylates with chiral Rh(I) complexes—comparison of phosphine ligands and substrates

The rhodium(I)-catalyzed enantioselective hydrogenation of E- and Z-configured β-acylamido β-alkylacrylates as well as of isomeric mixtures has been investigated. As ligands 1,2-bisphospholanes like DuPHOS, BPE and Me₄-BASPHOS have been tested, but also diphosphines forming seven-membered chelates such as DIOP. The effect of additional oxy groups in the diphosphine ligand on rate and enantioselectivity was likewise elucidated. In general, with all catalysts screened the hydrogenation is strongly sensitive to the E/Z-geometry of the substrate. E-Substrates are converted with good or excellent enantioselectivites into the desired β-amino acid derivatives. The hydrogenation of Z-substrates showed the known H₂-pressure dependency of the ee.     

冠醚－卟啉锰催化剂的制备及其催化性能研究

本文以一类新型的冠醚－卟啉作配体，制备了金属锰配合物．考察了该类配合物对苯乙烯环氧化反应的催化活性，发现具冠醚基团的锰卟啉催化剂在烯烃环氧化的两相溶剂（ＣＨ_２Ｃｌ_２／Ｈ_２Ｏ）体系中，不仅催化活性增强，同时具有相转移能力．本文还探索了反应条件改变对环氧化结果的影响规律，测定了反应的动力学．     

茂金属催化乙烯聚合反应动力学

以茂金属化合物[(CH3)2C(η－C5H3）（η－C9H6）]ZrCl2为主催化剂，甲基铝氧烷MAO为助催化剂催化乙烯聚合，对不同的反应条件下（如温度，铝锆摩尔比）聚合反应的动力学进行了研究，并根据此聚合反应体系的动力学特点及考虑到活性中心的再活化，在分析和研究以往的动力学模型的基础上，对烯烃均相聚合动力学反应作了一些假定，建立了动力学模型，用模型对实验数据进行了拟合，结果表明与实验数据相吻合，可以认为，在该聚合反应体系中，确实存在铝氧烷的再活化作用，根据模拟拟合得到了聚合反应的动力学参数。     

四元体系HCl-MClm-M′Cln-H2O中盐酸的活度系数 Ⅱ. HCl-KCl-BaCl2-H2O体系

从可逆电池H_2|HCl(I_1), KCl(I_2), BaCl_2(I_3)|AgCl-Ag的电位测定求得了在25 ℃时四元体系HCl-KCl-BaCl_2-H_2O中盐酸的活度系数γ_1。结果表明, 在恒定的总离子强度I及I_3条件下, 盐酸的的活度系数的对数亦随I_2线性地变化,但其数值比Harned在三元体系中所得到的对应数值略大一些, 和简单的1-1价硷金属卤化物四元体系中行为略为不同, 可能应表示为: logγ_1=logγ_(1(0))-a_(12)I_2-a_(13)I_3-K_(23)I_2I_3其中K_(23)为电解质2和3的作用系数。对我们所研究的体系, K的数值较小。初步的实验结果表明, 我们所推广的计算混介电解质活度系数的Glueckauf公式可以近似地应用于实际体系。应用热力学的交叉方程式于四元体系可以导出和前人在三元体系中所得到的一些相同的公式, 从这些式子有可能从实验的a_(12)、a_(13)数值求出a_(21)、a_(31)等数值。     

——>——>双核钴簇合物(C6H5CO2CH2C)2Co2(CO)6的合成与结构

The cluster (C_6H_5CO_2CH_2C)_2Co_2(CO)_6 has been synthesized and characterized by element analysis, IR, ~1H NMR etc. Its crystal structure has been determined by X-ray diffraction analysis with R=0.060. The crystal is triclinic, space group P_1 with a=0.8933(3) nm, b=1.1830(6) nm, c=1.3199(3) nm, α=65.64(3)°, β=84.55(3)°, γ=72.03(4)°, z=2, D_x=1.584 g cm~(-1) The C≡C and Co-Co form a tetrahedron with appoximate C_(2V) symmetry. The Co-Co bond is metl singal bond. The hybrid state of carbon atoms in the acetylene is between sp and sp~2.