环氧树脂/聚醚砜/纳米氧化铝复合材料的力学性能及介电性能

以甲基纳迪克酸酐（MNA）为固化剂,制备了环氧树脂/聚醚砜/纳米氧化铝三元复合材料,并对其力学性能、介电性能以及热稳定性能进行了研究,同时探讨了其性能增强机理。结果表明：当聚醚砜（PES）和纳米氧化铝（nano-Al₂O₃）的质量分数分别为15%和3%时,环氧树脂/15PES/3Al₂O₃复合材料的冲击强度、拉伸强度和弯曲强度分别达到45.7 kJ/m²、87 MPa和180 MPa,与纯环氧树脂相比,均有大幅度的提高。在测试频率为100 Hz时,复合材料的介电常数和介电损耗分别为7.7和0.013 5,介电性能较纯环氧树脂也有一定提高。此外,热分解温度比纯环氧树脂的提高了73℃,热稳定性得到提高。     

Fabrication of Durable Honeycomb‐Patterned Films of Poly(ether sulfone)s via Breath Figures

Honeycomb‐patterned porous films of poly(ether sulfone) (PES) are prepared via breath figures (BF), in which dichloromethane (DCM) is used as the solvent, although the solubility of PES in DCM is relatively low. It is found that the use of a DCM suspension of PES as the casting solution and the addition of an amphiphilic block copolymer, poly(styrene‐co‐maleic acid) partial isobutyl ester (PSME), assist the stabilization of water‐droplet arrays during the BF process, contributing to improved pattern regularity, and finally leading to the formation of highly ordered honeycomb‐patterned films of PES. A synergetic effect of concentration and humidity on the film morphology is discovered and systematically investigated. Moreover, the resultant films possess enhanced resistance to strong acid and base solutions under heating, indicating their promising applications under harsh conditions.

     

药用辅料二甲亚砜有关物质测定方法改进

摘 要 目的：参考各国药典对药用辅料二甲亚砜中有关物质的测定方法进行改进。 方法: 采用气相色谱法,以二苯甲烷为内标,Agilent DB wax毛细管柱（0.32 μm×30 m, 0.5 μm）,柱温:150℃,进样口温度:230℃,FID检测器温度:250℃,分流比：20∶1,进样量:2 μl。 结果: 在该色谱条件下,二甲亚砜中各杂质能完全分离;二甲基砜在6.58～526.50 μg·ml-1 的浓度范围线性关系良好（r=0.999 9）;平均回收率为101.27%（RSD=0.46%,n=6）。 结论: 本方法准确度高、重复性好,可用于二甲亚砜有关物质的测定。     

Ilaprazole,a new proton pump inhibitor,is primarily metabolized to ilaprazole sulfone by CYP3A4 and 3A5

1. Ilaprazole is a new proton pump inhibitor, designed for treatment of gastric ulcers, and developed by Il-Yang Pharmaceutical Co (Seoul, Korea). It is extensively metabolised to the major metabolite ilaprazole sulfone.

2. In the present study, several in vitro approaches were used to identify the cytochrome P450 (CYP) enzymes responsible for ilaprazole sulfone formation. Concentrations of ilaprazole sulfone were determined by liquid chromatography-tandem mass spectrometry (LC-MS/MS).

3. Incubation of ilaprazole with cDNA-expressed recombinant CYPs indicated that CYP3A was the major enzyme that catalyses ilaprozole to ilaprazole sulfone. This reaction was inhibited significantly by ketoconazole, a CYP3A inhibitor, and azamulin, a mechanism-based inhibitor of CYP3A, while no substantial effect was observed using selective inhibitors for eight other P450s (CYP1A2, CYP2A6, CYP2B6, CYP2C8, CYP2C9, CYP2C19, CYP2D6, and CYP2E1).

4. In addition, the formation of ilaprazole sulfone correlated well with CYP3A-catalysed testosterone 6β-hydroxylation and midazolam 1′-hydroxylation in 20 different human liver microsome panels. The intrinsic clearance of the formation of ilaprazole sulfone by CYP3A4 was 16-fold higher than that by CYP3A5.

5. Collectively, these results indicate that the formation of the major metabolite of ilaprazole, ilaprazole sulfone, is predominantly catalysed by CYP3A4/5.

     

1-[[4-(Aminoalkoxy)phenyl]sulfonyl]indolizines: a novel class of calcium entry blockers. Relationships between chemical structure, stereoelectronic properties and anticalcic activity

The solid-state structures of a series of 1-[[4-(aminoalkoxy)phenyl]sulfonyl]indolizines have been determined by X-ray analysis. These molecules are known to be representative of a novel class of calcium entry blockers characterized by a new binding site associated with the L-type calcium channel. Previous 2-dimensional structure-activity relationship studies have shown that 1-sulfonylindolizines substituted in the 2 position by an isopropyl group and possessing an aralkylamine substructure were among the most potent calcium antagonists. A comparative study of the 3-dimensional X-ray structures and the electronic properties computed at the ab initio HF level of five 1-sulfonyl, 2-alkyl and 2-phenylindolizine calcium antagonists presenting different types of amine substructures indicates important similarities within the series. This has led us to propose the first pharmacophoric elements for this kind of compound.     

莫达芬尼酸及莫达芬尼砜的核磁共振波谱研究

目的：对莫达芬尼酸和莫达芬尼砜进行核磁共振波谱(NMR)研究。方法：采用1D—NMR(^1H、^13C-NMR、DEPT)和2D-NMR(^1H-^1HCOSY、HMQC、HMBC)等现代核磁技术检测莫达芬尼酸和莫达尼酸的结构。结果：归属了莫达芬尼酸和莫达芬尼砜的H、C谱线。结论：首次报道了莫达芬尼酸和莫达芬尼砜的碳谱数据。     

Study on Chemical Cross-linking Modification of Hyaluronan and the Biocompatibility of its Derivatives

Objective: Prepare cross-linked HA gels with higher mechanical stability,lower degradation velocity and desirable biocompatibility,so as to extend the usage of HA.Method: 1.Test molecular weight of HA (MrHA) by viscosimetry;2.Prepare cross-linked HA gels by DVS,GTA,DEC;3.Discuss the cross-linking and degradation procedure;4,evaluate the biocompatibility of the best HA gels.Results: The mechanical stability and durability to degradation of HA-DVS gels are superior to those of other gels,and when HA :DVS = 40:1 (g/g),at 35℃ and in 0.2M NaOH solution,the HA-DVS gel shows the best mechanical stability,and its cytotoxicity reaches class I,hemolysis ratio is lower than 5 %.Conclusion:Our HADVS gel can be used to prepare biologic scaffolds.     

Base‐catalyzed deuterium and tritium labeling of aryl methyl sulfones

A method is presented for conveniently tritiating the aryl methyl sulfones of compounds identified as potent and selective inhibitors of human Cox‐2 and as DP receptor antagonists. A base‐catalyzed exchange reaction was conducted with deuterated water and the total deuterium incorporation, ranging from 46 to 99%, was calculated using mass spectrometry. Results from these exchanges were used as guidelines for tritium labeling giving specific radioactivities in the range of 28–120 mCi/mmol (1.03–4.43 GBq/mmol). Copyright © 2004 John Wiley & Sons, Ltd.     

Multicyclic Poly(ether sulfone)s Derived from Tris(4‐hydroxyphenyl)ethane

Polycondensations of 4,4′‐difluorodiphenylsulfone with tris(4‐hydroxy phenyl)ethane were performed in DMSO with variation of feed ratio and concentration. For feed ratios of 1.0:1.3–1.0:1.5, soluble multicyclic poly(ether sulfone)s were obtained when the monomer concentration was below 0.05 M . The conversions were never complete under standard conditions, and doubling the reaction time yielded perfect multicyclic products free of endgroups; however, a small fraction of the product was crosslinked under these conditions. Quite similar results were obtained with 4,4′‐dichlorodiphenylsulfone at higher temperatures. When K₂CO₃ was replaced by tertiary amines, conversions and molecular weights were lower. The multicyclic poly(ether sulfone)s were characterized by MALDI‐TOF mass spectrometry, SEC, and DSC measurements. Broad molecular weight distributions with polydispersities in the range of 2.4–3.9 were found, and, surprisingly, two glass transitions were detectable in the DSC heating curves.

     

聚醚砜-羟基磷灰石混合溶液的流变性能

采用N,N-二甲基乙酰胺(DMAc)为溶剂配制含羟基磷灰石(HAP)的聚醚砜(PES)溶液,研究了PES-HAP-DMAc体系的流变曲线以及HAP的质量分数、混合溶液温度等对流变性能的影响。结果表明：混合溶液的非牛顿指数（n）随着温度的升高、HAP质量分数的增大而降低,表现为非牛顿流体。