Novel preparation of organic polymer-based monolithic column by microwave irradation

Microwave irradiation was firstly attempted for the preparation of organic-based monoliths of poly（styrene-divinylbenzene- methacrylic acid）, which single step in situ polymerization was carried out during 15 min. The colunm permeability, electrophoretic and chromatographac behaviors were comparatively evaluated using pressure-assisted CEC, GEC and low pressure-driven separation modes. The largest theoretical plates for the preparing column could be close to 18,0000 plates/m for thiourea in the mode of p-CEC. It provided a viable alternative to traditional initiation means for the perparation of monolithic capillary columns.     

钴(Ⅱ)与5-(5-硝基-2-吡啶偶氮)-2,4-二氨基甲苯络合物吸附波及其应用

钴 (Ⅱ )在NH3·H2O -NH2OH·HCl-5_(5_硝基_2_吡啶偶氮)_2,4_二氨基甲苯体系中有一灵敏的极谱波 ,其峰电位Vp 为 -1.20V(vsSCE) ,钴质量浓度在0.25～25μg/L范围内与峰电流Ip′有良好的线性关系 ,检出限为0.12μg/L;经多种电化学方法证明该波为络合物吸附波 ,其电极过程为不可逆过程 ,电子转移数为2 ,此外还试验了多种离子对峰电流Ip′的影响;所拟方法已用于维生素B12 和模拟样中痕量钴的测定     

透射电镜像转角的测定及应用

论述了完全标定透射电镜像转角所需拍摄的二次曝光电子显微像的数量,推导了由已测的像转角间接计算其它像转角的一般公式,以Philips Cm200电镜为实例,说明了测定像转角的基本步骤,并以实例说明怎样利用像转角,把衍射花样的晶体学信息传递给电子显微像。     

5C + 1S] annulation: a facile and efficient synthetic route toward functionalized 2,3-dihydrothiopyran-4-ones

[reaction: see text] A facile and efficient synthetic route toward highly substituted 2,3-dihydrothiopyran-4-ones 2 has been developed via a formal [5C + 1S] annulation of readily available alpha-alkenoyl ketene-(S,S)-acetals 1 with sodium sulfide nonahydrated salt (Na2S x 9H2O) and utilized in the synthesis of 2-(4-chlorophenyl)-6-(morpholin-4-yl)-4H-thiopyran-4-one 5l, an inhibitor of DNA-dependent protein kinase (DNA-PK).     

Vacancy ion-exclusion chromatography of aromatic carboxylic acids on a weakly acidic cation-exchange resin

Determination of aromatic carboxylic acids by conventional ion-exclusion chromatography is relatively difficult and methods generally rely on hydrophobic interaction between the solute and the resin. To overcome the difficulties in determining aromatic carboxylic acids a new approach is presented, termed vacancy ion-exclusion chromatography, which is based on use of the sample as mobile phase and an injection of aqueous 10% methanol onto a weakly acidic cation-exchange column (TSKgel OApak-A). Highly sensitive conductivity detection occurred with sharp and well-shaped peaks, leading to very efficient separations. The effects of sulfuric acid concentration added to the mobile phase, flow-rate, and column temperature on the retention volume of tested aromatic carboxylic acids was investigated. Retention times were found to be affected by the concentration of the analytes in the mobile phase and to some extent also by the addition of an organic modifier such as methanol to the injected water sample. Separation of sulfuric acid (SA), naphthalenetetracarboxylic acid (NTCA), phthalic acid (PA) and benzoic acid (BA) was satisfactory using this new approach. Detection limits were 0.66, 0.67, 0.42 and 0.86 microM and detector responses were linear in the range 1-100, 1-80, 2.5-100 and 10-40 microM, for SA, NTCA, PA and BA, respectively. Precision for retention times was 0.36% and for peak areas was 1.5%.     

MALDI-TOF-MS法对重组人内皮抑素蛋白分子质量测定

肿瘤的生长依赖于血管的生成,新生血管不仅为肿瘤生长提供必需的营养物质,而且为肿瘤细胞扩散提供了重要的途径。1997年哈佛大学的O'Reilly等发现了一种内源性新血管生成抑制因子内皮抑素(Endoscatin),显示出特异抑制激活的血管内皮细胞增殖和肿瘤新血管生成的生物学活性,其抗肿瘤作用具有高效、低毒、无耐药性的优点。目前,内皮抑素的研究引起了国内外广泛的兴趣,在美国已进行以安全性为目的的I期临床实验,国内也有多家公司对内皮抑素进行了抗肿瘤研究并申报一类新药。内皮抑素有望成为医治肿瘤而又没有化疗和放疗的毒副作用的一种新的治疗方法,但是否能作为药物应用于临床,尚需对内皮抑素的结构特点及抑制肿瘤和内皮细胞的作用机制等方面进行许多深入的研究。     

Towards Single-component Molecular Conductor [Ni(dmit)_2] by Charge Disproportionation:2[Ni(dmit)_2]~(-0.5)[Ni(dmit)_2]+[Ni(dmit)_2]~-

It was commonly thought that a molecular conductor or semiconductor should be composed of at least two components to make the conducting component in partially charged state. However, this idea became questionable by the recent report of the single-component molecular conductor [Ni(tmdt)2]1 as well as several reports about single-component molecular semiconductors such as [Ni(ptdt)2]2 and [Ni(C10H10S8)2]3. In fact, as early as 1985, [Ni(dmit)2] as a by-product in synthesizing TTF[Ni(dmit…     

一类相变的Landau-deGennes模型——高斯近似

本文对一类相变的Landau-deGennes模型(以下简称L-deG模型)进行了高斯近似和平均场近似计算,获得一些“临界指数”的数值。例如,在高斯近似下,α=0.5≠α＇,γ=1≠γ＇,ν=0.5≠ν＇等等。我们计算了比热,并与液晶MBBA的实验进行了比较,讨论了向列相-各向同性液相相变与三重临界点的关系。文中特别着重讨论了一类与二类相变临界行为的异同。我们认为,二类相变的标度律结果不能简单地挪用到一类相变的情况。     

Ion chromatographic separation of hydrogen ion and other common mono- and divalent cations

We introduced an approach to the ion chromatographic determination of common mono- and divalent cations including hydrogen ion and demonstrated the ability of a C30 column dynamically coated first with dodecylsulfate and then with 18-crown-6 ether to separate the cations by ion-exchange mechanism. Using an ethylenediamine solution containing a small concentration of 18-crown-6 ether and lithium dodecylsulfate at pH 6.2 as eluent, the cations were eluted in the order Li < Na+ < NH4+ < H+ < K+ < Mg2+ < Ca2+ with symmetrical peaks. The conductivity vs. concentration plots were linear about three orders of magnitude, from millimolar to micromolar; and the detection limits were all < 0.6 microM. Rainwater was analyzed directly using this ion chromatographic system with satisfactory results.     

毒蕈碱受体激动剂的三维定量构效关系研究

采用比较分子场分析法(CoMFA)研究了55个四氢吡啶类毒蕈碱受体激动剂的三维定量构效关系(3D-QSAR), 建立了具有较强预测能力的3D-QSAR模型. 所得模型的交叉验证相关系数(q²)为0.507, 常规相关系数(R²)为0.982 , 标准方差为0.218, 说明系列化合物分子周围立体场和静电场的分布与生物活性间存在良好的相关性. 模型不仅很好地预测了训练集和测试集化合物的活性, 而且为设计活性更高的受体激动剂提供了理论依据.