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991.
基于戊二醛具有双官能团、高反应活性的特征,以其为间隔臂将万古霉素键合到氨基二氧化硅填料表面,制备了万古霉素键合手性固定相,制备方法简单易行。采用元素分析及扫描电子显微镜对制备的万古霉素键合手性固定相进行了表征。在高效液相色谱分离模式下,分别对谷氨酸、天冬氨酸、苯丙氨酸和异亮氨酸等4种手性氨基酸和手性药物罗格列酮进行拆分,其中谷氨酸和罗格列酮的分离度分别达到了2.0和2.3。系统考察了流动相条件对对映体拆分的影响,证实有机改性剂、缓冲液种类和浓度、pH值及温度对所测样品的保留行为和手性选择性均有显著影响。 相似文献
992.
采用高效液相色谱-电喷雾-离子阱质谱法(HPLC-ESI-IT-MSn)对硫酸依替米星中有关物质结构进行推定.采用Phenomnex Gemini NX C18色谱柱,以水-氨水-冰醋酸(96∶ 3.6∶ 0.4, V/V)-甲醇(70∶ 30, V/V)为流动相,质谱条件:电喷雾离子源(ESI),正离子检测模式;离子源温度350 ℃;雾化氮气压力275.8 kPa;干燥氮气流速10 L/min;离子阱质谱检测器,Smart扫描模式,扫描质量范围m/z 100~900.硫酸依替米星样品中共检出18种有关物质,对其中的13种物质的结构进行了推定,其余5种有关物质的结构未进行解析,只提供了分子量和二级质谱信息. 相似文献
993.
994.
Yibo Lei Bingbing Suo Yusheng Dou Yubin Wang Zhenyi Wen 《Journal of computational chemistry》2010,31(8):1752-1758
Multireference configuration interaction with single and double excitations (MRCISD) as well as its analytic CI gradients has been implemented in the semiempirical framework. The hole‐particle symmetry and a mixed driven model for computing coupling coefficients have been used in the new code that allows us to perform MRCI and gradient calculations with higher efficiency and less storage requirements. © 2010 Wiley Periodicals, Inc. J Comput Chem, 2010 相似文献
995.
Hiromasa Aono Dingy Wen Li Zang Damian Houde R. Blake Pepinsky David R.H. Evans 《Journal of chromatography. A》2010,1217(32):5225-5232
Protein trisulfide linkages are generated by the post-translational insertion of a sulfur atom into a disulfide bond. Molecular heterogeneity was detected in a recombinant IgG1 monoclonal antibody (mAb) and attributed to the presence of a protein trisulfide moiety. The predominant site of trisulfide modification was the bond between the heavy and light chains. The trisulfide was eliminated during purification of the IgG1 mAb via a cysteine wash step incorporated into Protein A affinity column chromatography. Analysis of the cysteine-treated mAb by electrophoresis and peptide mapping indicated that the trisulfide linkages were efficiently converted to intact disulfide bonds (13% trisulfide decreased consistently to 1% or less) without disulfide scrambling or an increase in free sulfhydryls. The on-column trisulfide conversion caused no change in protein folding detectable by hydrogen/deuterium exchange or differential scanning calorimetry. Consistent with this, binding of the mAb to its antigen in vitro was insensitive to the presence of the trisulfide modification and to its removal by the on-column cysteine treatment. Similar, high efficiency trisulfide conversion was achieved for a second IgG1 mAb using the column wash strategy (at least 7% trisulfide decreased to 1% or less). Therefore, trisulfide/disulfide heterogeneity can be eliminated from IgG1 molecules via a convenient and inexpensive procedure compatible with routine Protein A affinity capture. 相似文献
996.
Self Microemulsifying Drug Delivery Systems (SMEDDS) are a novel alternative to the conventional transdermal delivery systems. SMEDDS are water-free systems, made up of oils and surfactants that can readily form a microemulsion upon dilution within an aqueous medium. Before SMEDDS can be used as a drug delivery system it is necessary to investigate the internal microstructure of the resulting microemulsion. Novel Imwitor 308 based SMEDDS were prepared and investigated. Phase behaviour of the comprising components was investigated through the construction of pseudoternary phase diagrams. The formed systems were characterized using visual inspection, measurement of electrical conductivity, viscosity and droplet size. Amongst the pseudoternary systems investigated, IPM/Cremophor EL (50% w/w)/Imwitor (50% w/w) and Myritol 318/Tween 85 (64% w/w)/ Transcutol P (20% w/w)/Imwitor (16% w/w) possessed the largest microemulsion area. Electrical conductivity and viscosity studies depict structural transitions from w/o microemulsion to bicontinuous or o/w microemulsion around 20-35% water. This was further supported by the droplet size and Fourier transform (FT)-IR measurements. The FT-IR data suggests that below the percolation threshold (ψ(C)) the water molecules are mainly bounded to the surfactant head group (bound water). Above this value, water molecule move to the outer phase of the microemulsion mainly interacting with each other though hydrogen bounding (free water). It was also found that pseudoternary systems with water content of less than 30% were stable at 32°C. Such systems may form stable microemulsion upon contact with the skin. Absorption of water may also result in a supersaturated solution with enhanced transdermal flux. 相似文献
997.
Sun HY Xiao CF Cai YC Chen Y Wei W Liu XK Lv ZL Zou Y 《Chemical & pharmaceutical bulletin》2010,58(11):1492-1496
The practical synthesis of important natural polyphenolic stilbenes, including resveratrol, piceatannol and oxyresveratrol, through Perkin methodology is described. Starting from 3,5-dihydoxyacetophenone (1), the common intermediate 3,5-dimethoxyphenylacetic acid (3) can be obtained via methylation and Willgerodt-Kindler reaction. Perkin condensations between (3) and substituted phenylaldehydes 4 furnished E-2,3-diarylacrylic acids 5, followed by decarboxylation in Cu/quinoline giving stilbene intermediates 6 which bear the Z-configuration. Finally, through a simultaneous demethylation/isomerization process in AlI?/CH?CN system, the target compounds 7a-c can be obtained respectively in good to high overall yields. The synthetic method proved to be more concise, trans-specific, mild, economical and commonly applicable. 相似文献
998.
Synergistic antitumor effect of curcumin and dinitrosyl iron complexes for against melanoma cells 总被引:1,自引:0,他引:1
Yu-Der Wen Rong-Jen Shiau Jheng-Yu Wu Show-Jen Chiou 《Journal of organometallic chemistry》2010,695(3):352-1579
The aim of this study was to examine whether combining curcumin, a chemoprevention agent, and dinitrosyl iron complexes (DNICs) would have a synergistic cytotoxic effect on mouse melanoma B16-F10 cells in vitro. Three synthesized DNICs-[PPN] [(NO)2Fe(SCH2CONHCH3)2] (NC01), [PPN] [(NO)2Fe(SCH2CON(CH3)2)2] (NC02), and [Na][(NO)2Fe(SCH2CON(CH3)2)2] (NC03) were tested in this study. In vitro DNA cleavage assay showed all three DNICs could cause plasmid DNA damage through releasing NO under UV irradiation. The cytotoxicity assay demonstrated these DNICs were toxic to B16-F10 cells in vitro, and the estimated values of LD50 (24 h of incubation) of NC01 and NC02 were 1 μM, while the values of LD50 of NC03 was 200 μM. No synergistic cytotoxicity effect was noted in the treatments of the combinations of curcumin and DNICs. On the contrary, in the presence of NC03, the toxicity of curcumin was reduced. Using UV-Visible spectroscopy and fluorescence microscopy, we found NC03 might interact with curcumin and reduce the accumulation of curcumin in cells. Further experiments using the pretreatment of curcumin for 4 h followed by the treatment of NC03 showed the synergistic cytotoxic effect, while, the pretreatment of NC03 followed by the treatment of curcumin did not have any effect. This study provides the basis for further investigation on the effects of combinations of curcumin and other NO donors. 相似文献
999.
Zhang AH Jiang N Gu W Ma J Wang YR Song YC Tan RX 《Chemistry (Weinheim an der Bergstrasse, Germany)》2010,16(48):14479-14485
(-)-Alternarlactam [(-)-1], a new promising cytotoxin against two human cancer cell lines, was isolated from an endophyte culture and synthesized (along with (+)-1) from readily available starting materials. The absolute configuration, chirality-activity relevance and self-aggregation of (-)-1 were assigned by a combination of synthetic, spectroscopic and computational approaches. The full characterization of the new fungal cytotoxin may provide valuable information in the discovery of new antitumor agents. 相似文献
1000.
Wen‐Yong Lai Dr. Ruidong Xia Dr. Donal D. C. Bradley Prof. Dr. Wei Huang Prof. Dr. 《Chemistry (Weinheim an der Bergstrasse, Germany)》2010,16(28):8471-8479
We present herein a novel design and the efficient synthesis towards a “homogeneous” starburst fluorene system based on the novel 2,3,7,8,12,13‐hexaaryltruxene scaffold. Controlled microwave heating provides a facile and powerful approach for each step in the synthesis of these bulky materials with large steric hindrance, suggesting an avenue to access structurally well‐defined complex organic semiconductors (OSCs) rapidly and conveniently with high yield and purity. The resulting materials exhibited good thermal stability and an excellent glassy structure as revealed by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) as well as wide‐angle X‐ray diffraction (WAXD) studies. Moreover, compared with their corresponding three‐arm‐substituted counterparts T1 – T4 , the introduction of the ortho substituents around the truxene core in Tr1 – Tr4 results in significant blueshifts (of 7–24 nm) of the absorption maxima λmax and higher energy optical gaps (Eg). Comparative studies with corresponding linear, rod‐shaped oligofluorene counterparts (OFX) have revealed that the longest para‐conjugated segment in the TrX (X=1–4) structures plays the dominant role in determining their electronic properties. UV/Vis data and cyclic voltammetry (CV) investigations have indicated that there is little electronic interaction between the arms, even for the shortest armed oligomer Tr1 . A clear linear relationship of both 1/λmax and Eg with the inverse of (n+1) for these branched systems was found. Our findings highlight a novel molecular design comprising an ortho‐substituted, multiarmed architecture that would allow the introduction of isotropic physical and/or mechanical properties, while at the same time maintaining most of the important electronic properties of the rod‐shaped constituents of a fully conjugated system. 相似文献