Application of silver staining to the rapid typing of the polymorphism of HLA-DQ alleles by enzymatic amplification and allele-specific restriction fragment length polymorphism.

A rapid and highly sensitive silver staining method, originally developed for the detection of proteins, was slightly modified to detect nucleic acids in polyacrylamide gels. The second exons of the histocompatibility antigen HLA-DQA 1 and DQB 1 genes were selectively amplified from genomic DNA by the polymerase chain reaction (PCR). Digestion of the PCR products by endonucleases, followed by their size-separation on polyacrylamide gels and visualization by silver staining, allowed us to define the HLA-DQ alleles of the genomic DNA. The intensity of staining of digested PCR-amplified DNA is linear from at least 8 to 18 ng for fragments of lengths ranging from approximately 40 to 200 bp. Thus, silver staining in combination with PCR and allele-specific restriction fragment length polymorphism provides a simple, safe, and rapid method for accurate definition of HLA-DQ alleles at the nucleotide level in the clinical typing laboratory.     

Determination of copper in white-metal bearing alloys

A method is proposed for the determination of copper in white-metal bearing alloys by direct controlled-potential electrolysis with a tantalum cathode at -0.32 V vs. SCE in a sulphate/bisulphate buffered electrolyte (pH 2) with fluoroboric acid and sodium tartrate as masking agents. Only Bi(III) interferes. Any co-deposited Bi can be corrected for by its spectrophotometric determination with Semi-Xylenol Orange after preconcentration with La(III) as carrier, from an ammoniacal solution containing the redissolved deposit. Any residual Cu(II) in the electrolyte is determined by spectrophotometry with 2,9-dimethyl-1, 10-phenanthroline. The standard deviation of this method has been found to be 0.03 mg (n = 12) and its relative standard deviation from 0.03 to 0.17%. It has been successfully used for referee analysis and certification of standard reference materials.     

Coordination geometries and cooperative ordering effects in copper(II) complexes with tridentate Schiff base dianions 5 E.p.r. spectra of [N-salicylidene-(R,S)-alaninato]copper(II) complexes with derivatives of imidazole and pyrazole and structure of 1-methylimidazole[N-salicylidene-(R,S)-valinato]copper(II)

1-Methylimidazole[N-salicylidene-(R,S)-valinato]copper(II) shows square-planar coordination around the Cu2+ ion, coordinated in the basal plane by O,N,O atoms from the tridentate Schiff base dianion and by N from the coordinated 1-methylimidazole. In the crystal structure, enantiomers related by an inversion centre are bound by H bonds to units with a CuCu distance of 8.039Å. Intermolecular H bonds stabilize stacking of such units, which are propagated along the [010] axis. Two such chain systems in the unit cell are related by a glide plane parallel to (010). The basal planes of two magnetically non-equivalent complexes are canted by an angle of 74.64. The shortest CuCu distance between non-parallel-aligned coordination polyhedra is 10.518Å. On the other hand, the closest CuCu spacing of parallel-orientated coordination polyhedra is 5.628Å. Hence, in the e.p.r. powder spectrum only the coupling between ferrodistortively ordered coordination polyhedra is manifested.E.p.r. and ligand field spectra of a series of [N-salicylidene-(R,S)-alaninato]copper(II) complexes with imidazole, pyrazole and some of their derivatives provide evidence for coordination geometries ranging from square-pyramidal, with various strengths of axial interaction, to square-planar. The cooperative ordering phenomena in the structure are discussed on the basis of the e.p.r. powder spectra. When the e.p.r. spectra yield crystal g values from two coupled molecular g tensors of orthorhombic symmetry, a simple model based on consistency of G parameters was developed for evaluation of the canting angle 2 between aligned coordination polyhedra and molecular g values, respectively. The data obtained from the e.p.r. powder measurements are in excellent agreement with the results of single X-ray structural studies.     

血红蛋白的同步荧光光谱随浓度变化的特性

报道了血红蛋白的同步荧光光谱，研究了血红蛋白浓度浓度对光谱的影响，确认了血红蛋白四聚体和二聚体的特征光峰。     

氧化铝基COS、CS_2水解催化剂表面碱性和催化作用

进行了３种氧化铝基催化剂上ＣＯ２的ＴＰＤ和ＣＯＳ、ＣＳ２的水解活性研究．结果表明，催化剂表面碱性中心类型、强度和数目是不相同的；Ｋ２Ｏ和Ｐｔ的负载能提高弱碱性中心的数目和强度，同时能显著提高ＣＯＳ、ＣＳ２的水解转化率．关联第一类ＣＯ２脱附活化能和峰面积与ＣＯＳ水解反应活化能和速率常数，发现呈线性关系，说明弱碱性中心是ＣＯＳ催化水解的活性中心．关联第一、二两类ＣＯ２脱附峰面积与ＣＳ２水解速率常数，指出弱、次弱两类碱性中心均参与了ＣＳ２催化水解．催化剂表面上能量的分布是不均匀的．     

凝胶化反应全过程的激光光散射跟踪研究

在苯乙烯（Ｓｔ） 二乙烯苯（ＤＶＢ）自由基共聚的凝胶化反应过程中定时取样，得到凝胶化点前后及至终点的一系列样品，然后用激光光散射技术，包括研究散射光强及其角度依赖性的静态光散射（ＳＬＳ）和研究散射光频移的动态光散射（ＤＬＳ），表征了这系列样品的重均分子量Ｍｗ、均方旋转半径Ｒｇ、第二维利系数Ａ２及流体力学半径Ｒｈ等静、动态参量及这些参量的变化规律，定量地描述了凝胶化反应全过程     

The tautomerism of 6-hydroxy-, 6-amino- and 6-acylamino-7-azaindolines

The lactam-lactim tautomerism of 6-hydroxy-7-azaindolines and amino-imine tautomerism of 6-amino- and 6-acylamino-7-azaindolines has been studied by IR and UV spectroscopy. It is shown that the lactam-lactim tautomeric equilibrium of 6-hydroxy-7-azaindolines in contrast to the other analogous N-heteroaromatic compounds is not completely shifted for the lactam. The commensurable amounts of both tautomeric forms can be observed in the solutions of 6-hydroxy-7-azaindolines and it is possible to elucidate the influence of the solvent polarity upon the lactam-lactim tautomeric equilibrium. The tautomeric equilibrium of 6-amino- and 6-acylamino-7-azaindolines is practically completely shifted for the amino form, and even acylation with p-toluene-sulfonic acid does not result in a noticeable shift of the tautomeric equilibrium for the amino form in contrast to the other N-heterocyclic amines.     

酪氨酸激酶抑制剂的三维定量构效关系研究

利用柔性原子受体模型(FLARM)方法对一系列的异黄酮和喹诺酮衍生物表皮生长因子受体酪氨酸激酶抑制剂进行了三维定量构效关系研究，得到了合理的构效关系模型.FLARM方法的计算结果还给出了虚拟的受体模型，该模型说明了抑制剂与受体之间可能的相互作用.由该虚拟受体模型得到的受体-配体相互作用与Novartis药效团模型比较类似.     

A new titanium tetrachloride mediated annulation of alpha-aryl-substituted carbonyl compounds with alkynes: A simple and highly efficient method for the regioselective synthesis of polysubstituted naphthalene derivatives

A new straightforward procedure has been developed for the synthesis of polysubstituted naphthalene derivatives. The reaction of alpha-aryl-substituted carbonyl compounds with terminal or internal alkynes in the presence of TiCl4 regioselectively generates substituted naphthalene derivatives in good to excellent yields.     

Regioselective construction of polysubstituted phenols from Baylis-Hillman adducts via formal [4+2] annulation strategy

Polysubstituted phenol derivatives were synthesized regioselectively starting from the Baylis-Hillman adducts via the formal [4+2] annulation protocol as the key step.