促δ-波睡眠肽的结构与功能的研究

用固相法合成了促δ-波睡眠肽Trp-Ala-Gly-Gly-Asp-Ala-Ser-Glu(DSIP)及其十四种类似物和三个短肽,研究了结构与功能的关系,类似物的设计,主要考虑在分子中引入D-氨基酸以抑制酶的作用和增强稳定性,以及引入疏水侧链氨基酸如Phe和Trp等。位置的修饰主要在1,3,4,5,8和9位,即:D-Trp[1],Tyr[1],Tyr[1]Phe[5],D-Trp[1]Phe[8],Trp[3,4],D-Trp[3,4],D-Trp[1,3,4]Phe[8],D-Glu[9],D-pF-Phe[3,4]Phe[8]D-Glu[9],Phe[5],Glu[5]Asp[9],Tyr[5]Asp[9],Ala[7]和Asp[9]-DSIP以及Trp-Ala-Gly-Gly-Asp,Trp-Ala-Gly-Gly-Glu和Trp-Gly-Glu.合成肽的纯度经氨基酸组成分析、元素分析、薄层层析以及纸电泳鉴定。生物试验表明D-Trp[1],Tyr[1],Tyr[1]Phe[5],Ala[7]-DSIP无促眠活性;而Phe[5]-DSIP的促眠活性与DSIP相接近,其他类似物的生物试验结果将另文发表。     

Synthesis and Crystal Structure of 9-（ 4-M e tho xylphen yl ）-1,8-dioxo-3,4,5,6,7,9hexahydroxanthene under Microwave Irradiation

1INTRODUCTIONInthepastfewyears,potassiumchannelacti-vatorshavegainedincreasingattentionbecauseoftheirclinicalpotentialapplicationsinvariousdiseases.Oneofthemostpotentcompoundsamongthisnewclassofdrugsisthebenzopyranderivativecroma-kalim[1～4].Benzopyranaswellasitsderivativesex-hibitsextensivepharmacologicalandbiologicalacti-vities[5],suchasantibacterialactivities[6,,antitumor7]activity[8],hypotensiveeffect[9],antiproliferationef-fect[10],etc.Thetitlecompoundbearingabenzo-pyranstructuraluni…     

亚甲基[6,6]-富勒(fullerene)[60]单羧酸的合成研究

亚甲基[6,6]-fullerene[60]单羧酸是一个具有化学反应活性的fullerene[60]衍生物,可以作它合成得到一些新的具有潜在生化应用价值的水溶性fullerene[60]衍生物。本文详细报道了常规量合成亚甲基[6,6]-fullerene[60]单羧酸的技术。     

溴邻苯三酚红双波长分光光度法测定铝合金中铜北大核心CSCD

在铝合金中加入铜,能增加铝合金的强度,提高铝合金的应力腐蚀抗力,因此测定铝合金中铜的含量具有重要意义。溴邻苯三酚红是一种重要的显色试剂,已用于羟自由基[1]、碘[2]、蛋白质[3]、乙二胺四乙酸（EDTA）[4]、钼[5]、硒[6]、铌[7]、铝[8]等的测定。双波长分光光度法在光度分析中的应用较为广泛[9-10]。     

Three New Silver Alkylenediphosphonates with Pillar-like Open-frameworks

1 INTRODUCTION From 1970s many research interests have focused on metal organophosphonates due to their structural diversities, including layers[1, 2], zeolite-like[3], inor- ganic channel with organic shell[4], cage-like[5], homo- chiral framework[6] and ring-[7] or sphere-like[8] clus- ters, as well as their potential or practical applica- tions as Langmuir-Blodgett Film (LB)[9], meso/mi- cro-porous materials[10, 11], ion-exchangers [12], small molecular sensors[13], adsorptions/desorp…     

溶剂热法制备钴微球及其表征

<正>0引言过渡金属钴以及它的一些氧化物,以其特殊的电、磁和光学性能被广泛应用到信息存储[1]、催化剂[2]、磁光材料[3]、铁磁流体[4]以及生物医学[5]等诸多领域。前人曾经用羰酰钴热解法[6-7]、γ射线照射法[8]、光刻气相沉积法[9]、电化学沉积法[10]和金属盐溶液的     

铑催化环加成反应的研究进展

综述了近几年铑催化剂在环加成反应中的研究进展, 主要包括[2＋2], [2＋2＋1], [2＋2＋2], [3＋2], [3＋4]和[4＋2]环加成反应等, 讨论了铑催化下的环加成反应及其机理.     

Synthesis and Characterization of Rh—Co Butterfly Clusters Capped by Functionally Substituted 1—Alkynes

1INTRODUCTIONThemixed-transition-metalclustershavehighpotentialtoserveasefficientcatalystsforavarietyofhomogeneouscatalyticreactionsaswellasuniquereagentsfororganicsyntheses[1].Ithasbeenreportedthatthereactionsof[Rh2Co2(CO)12]withseveralalkynestogiveRh-Comixed-metalbutterflyclusters[1～4].Inaddition,thereactionofsilylformylationof1-hexynewiththehydro-formylationofcyclohexene,1-penteneandstyrenehavealsobeeninvestigatedbyusing[Rh2Co2(CO)ascatalyst[5].Inordertogainmoreunderstandingaboutt…     

Synthesis and Crystal Structure of Ethyl 5-Amino-1-[（5′-methyl-1′- t-butyl-4′-pyrazolyl）carbonyl]-3-methylthio-1H-pyrazole-4-carboxylate

1INTRODUCTIONPolarizedketenedithioacetalshavebeenex-tensivelyusedasbuildingblocksinorganicsyn-thesis,especiallyinthesynthesisofheterocycliccompounds[1～6].Pyrazoleanditsderivativesrepre-sentoneofthemostactiveclassesofcompoundspossessingwidespectraofbiologicalactivities.Overthepastfewyears,considerableevidenceshavebeenaccumulatedtodemonstratetheefficacyofpyrazolederivatives,suchasantibacterial[7],fun-gicidal[8],herbicidal[9],insecticidal[10]andotherbiologicalactivities[11,12].Uptonow,alarg…     

阻抑光度法测定痕量铁(Ⅲ)

铁是人体不可缺少的微量元素,是血红蛋白的核心部分,正常成人体内铁的总量为2~4g。目前,测定痕量铁的方法有伏安法[1]、化学发光法[2]、色谱法[3]、极谱法[4]、原子吸收光谱法[5]、激光光热折射光谱法[6]、微晶石蜡柱固相萃取法[7]、二阶导数光谱-峰面积积分光度法[8]和分光光度法[9]等。阻抑动力学分光光度法是利用具有氧化性的物质如高碘酸钾、过氧化氢、三价铁离子、溴酸钾等,对在不同波     

Red phosphorus acts as second acid source to form a novel intumescent-contractive flame-retardant system on ABS

A novel halogen-free flame retardant prepared by poly(p-ethylene terephthalamide) and ammonium polyphosphate (APP) on acrylonitrile–butadiene–styrene (ABS) resin has a good flame retardancy when loading is 30 %; but, once the mass fraction is <30 %, the system does not maintain outstanding flame retardancy. To improve the efficiency of this kind of flame retardant and LOI values, higher thermal stability acid source-red phosphorus is introduced. It is found that a little quantity of red phosphorus will improve the flame retardancy of ABS remarkably and will change the process of charring; when the mass fractions of APP, PPTA, and red phosphorus are only 15, 5, and 2 %, respectively, though the LOI of flame-retardant ABS is 27, UL-94 vertical burning test still reach V-0. Thermogravimetric analysis data show that red phosphorus changes the thermal degradation behavior of IFR-ABS system, shrink digital photo display system, and yield more stable residue at higher temperature; Fourier transform infrared results and scanning electron microscopic micrographs show that red phosphorus can catalyze the charring and form much denser char to improve the flame-retardant performance of the materials.     

Effect of a novel charring agent on thermal degradation and flame retardancy of acrylonitrile–butadiene–styrene

A novel charring agent poly(p-propane terephthalamide) (PPTA) was synthesized by using terephthaloyl chloride and 1,3-propanediamine through solution polycondensation and it was used together with ammonium polyphosphate (APP) to prepare a novel intumescent flame retardant (IFR) for ABS. The thermal degradation behaviour and flame retardancy were investigated, the results showed that PPTA could be effective as a charring agent, the flame retardancy of ABS and the mass of residues improved greatly with the addition of IFR. When the content of APP was 22.5 mass% and PPTA was 7.5 mass%, the limiting oxygen index (LOI) value of IFR-ABS system was found to be 32.4, and class V-0 of UL-94 test was passed. Moreover, the synergistic effects of two different adjuvants AlPi and MnO₂ in IFR-ABS system have been studied.     

Towards the development of thermally latent novolac-based char formers for ABS resins

Novel novolac-based char formers for ABS resins, [PN-PI], [PN-BPI], [CN-PI] and [CN-BPI], were prepared from phenol formaldehyde novolac (PN), cresol formaldehyde novolac (CN), phenyl isocyanate (PI), and 4-biphenyl isocyanate (BPI) via a simple urethane-forming reaction. The four compounds were used as thermally latent char formers for this study. Thus, a two component system employing novolac-isocyanate adduct as a char former, and tetra-2,6-dimethyl phenyl-resorcinol diphosphate (DMP-RDP) as a phosphorous-based flame retardant was blended with ABS, and the thermal degradation behaviour and flame retardancy were determined by thermogravimetric analysis (TGA) and LOI test. The mixtures show a synergistic effect between DMP-RDP and novolac-isocyanate adduct on the flame retardance enhancement of ABS. Those containing higher molar mass CN-BPI adduct are found to be most flame retardant, and a LOI value as high as 35 is obtained.     

A novel halogen-free flame retardant for glass-fiber-reinforced poly(ethylene terephthalate)

In order to prepare halogen-free flame-retardant glass-fiber-reinforced poly(ethylene terephthalate) (FR-GF-PET), a novel flame retardant containing three flame-retardant elements, P, N and S, was synthesized by melt condensation reaction. Its chemical structure was characterized by FT-IR and ¹H NMR spectra. FR-GF-PET was prepared by melt-mixing the flame retardant with GF-PET. The effects of the flame retardant on the flammability and thermally decomposing behaviors of GF-PET were studied via LOI, UL-94 and TGA tests. The results showed that despite a negative effect on the thermal stability of GF-PET, the incorporation of the flame retardant improved the flame retardancy of GF-PET largely. The LOI values of GF-PET increase linearly with the increase of flame retardant content. The GF-PET passed the V-0 rating in UL-94 tests when 15 wt% of the flame retardant was added to GF-PET. An interesting phenomenon was found, that is, with the increase of flame retardant content, the flame retardancy of the system increased but the char yield decreased, which was explained according to the evidences of XPS tests and the kinetics of thermally decomposing reaction.     

Synthesis of functionalized α-zirconium phosphate modified with intumescent flame retardant and its application in poly(lactic acid)

A novel functionalized α-zirconium phosphate (F-ZrP) modified with intumescent flame retardant was synthesized by co-precipitation method and characterized. Poly (lactic acid) (PLA)/F-ZrP nanocomposites were prepared by melt blending method. The thermal stability and combustion behavior of PLA/F-ZrP nanocomposites were investigated by thermogravimetric analysis (TGA), limiting oxygen index (LOI), vertical burning test (UL-94), scanning electronic microscopy (SEM), and cone calorimeter test (CCT). The results showed that the addition of flame retardant F-ZrP slightly affect PLA's thermal stability, but significantly improve the flame retardancy of PLA composites. In comparison with neat PLA, the LOI value of PLA/F-ZrP was increased from 19.0 to 26.5, and the UL-94 rating was enhanced to V-0 as the loading of F-ZrP at 10%. SEM results suggested the introduction of F-ZrP in the PLA system can form compact intumescent char layer during burning. All these results showed that the F-ZrP performed good flame retardancy for PLA.     

Flame‐retardancy and anti‐dripping effects of intumescent flame retardant incorporating montmorillonite on poly(lactic acid)

In the present study, the effects of intumescent flame retardant (IFR) incorporating organically modified montmorillonite (O‐MMT) on the flame retardancy and melt stability of PLA were investigated. The flame‐retardant PLA was prepared using a twin‐screw extruder and a two roll mill. Then, the influence of IFR and MMT on flame retardancy and melt stability was thoroughly investigated by means of limiting oxygen index (LOI), vertical burning test, thermogravimetric analysis, scanning electronic microscopy, melt flow index (MFI), and parallel plate rheological experiments. The experimental results show that the IFR system in combination with MMT has excellent fire retardancy, i.e. the sample could achieve a UL94 V‐0 rating and LOI value increases from 20.1 for pristine PLA to 27.5 for the flame‐retarded PLA. MFI and rheological measurement indicate that O‐MMT significantly enhances the melt stability and suppresses the melt dripping. Copyright © 2009 John Wiley & Sons, Ltd.     

次磷酸铝协同硼酸锌阻燃聚乙烯

以次磷酸铝(AHP)和硼酸锌(ZB)为复合阻燃剂,通过熔融共混法制备了阻燃聚乙烯(PE)材料,研究了AHP和ZB对PE的协同阻燃效应。 结果表明,AHP、ZB阻燃剂在PE基体中分散均匀;添加质量分数为25%AHP阻燃剂,PE材料的极限氧指数值(LOI)提升至25%,通过垂直燃烧测试(UL-94(3.2 mm))V-2级,显示出良好的阻燃效果;引入ZB后,材料LOI值呈先升高后下降趋势,在m(AHP):m(ZB)=21:4时,出现峰值,达到27.2%,并通过UL-94(3.2 mm)V-1级;热失重分析(TGA)结果显示,AHP、ZB阻燃剂能同时提高PE材料的热稳定性和成炭率,当m(AHP):m(ZB)=17:8时,残渣率达到25.7%。     

Synergistic effect of boron containing substances on flame retardancy and thermal stability of clay containing intumescent polypropylene nanoclay composites

The functions of nanoclay and three different boron containing substances, zinc borate (ZnB), borophosphate (BPO₄), and boron silicon containing preceramic oligomer (BSi), were studied to improve the flame retardancy of polypropylene (PP)‐nanoclay‐intumescent system composed of ammonium polyphosphate (APP) and pentaerythritol (PER). The flame retardancy of PP composites was investigated using limiting oxygen index (LOI), UL‐94 standard, thermogravimetric analysis (TGA), and cone calorimeter. According to the results obtained, the addition of 20 wt% intumescent flame retardant (IFR) improved the flame retardancy by increasing the char formation. Addition of clay slightly increases the LOI value and reduces the maximum heat release rate (HRR). Addition of clay also increases the barrier effect due to intumescent char, especially in thin samples. Boron compounds show their highest synergistic effect at about 3 wt% loading. According to UL‐94 test and LOI test, 3 wt% ZnB containing composite shows the highest rating (V0) and BPO₄ containing sample shows the highest LOI value (26.5). Copyright © 2010 John Wiley & Sons, Ltd.     

Intrinsically flame retardant epoxy resin - Fire performance and background - Part I

The flame retardant effect of newly synthesized phosphorus-containing reactive amine, which can be used both as crosslinking agent in epoxy resins and as a flame retardant, was investigated. The effect of montmorillonite and sepiolite additives on the fire induced degradation was compared to pristine epoxy resin. The effect of combining the organophosphorous amine with clay minerals was also studied. It could be concluded that the synthesized phosphorus-containing amine, TEDAP can substitute the traditional epoxy resin curing agents providing additionally excellent flame retardancy: the epoxy resins flame retarded this way reach 960 °C GWFI value, 33 LOI value and V-0 UL-94 rating - compared to the 550 °C GWFI value, 21 LOI value and “no rate” UL-94 classification of the reference epoxy resin. The peak of heat release was reduced to 1/10 compared to non-flame retarded resin, furthermore a shift in time was observed, which increases the time to escape in case of fire. The flame retardant performance can be further improved by incorporating clay additives: the LOI and the HRR results showed that the optimum of flame retardant effect of clay additives is around 1 mass% filler level in AH-16-TEDAP system. Applying a complex method for mechanical and structural characterization of the intumescent char it was determined that the flame retarded system forms significantly more and stronger char of better uniformity with smaller average bubble size. Incorporation of clay additives (owing to their bubble nucleating activity) results in further decrease in average bubble diameter.     

The application of Ce‐doped titania nanotubes in the intumescent flame‐retardant PS/MAPP/PER systems

In this work, we reported the synthesis, characterization of Ce‐doped titania nanotubes (Ce‐TNTs), and application in flame retardancy of an intumescent flame‐retardant polystyrene (PS/IFR) system. The flame retardancy of polystyrene (PS) composite that was composed of pentaerythritol, microencapsulated ammonium polyphosphate, and PS was enhanced significantly by adding a small amount (0.1 wt%) of (Ce‐TNTs). The thermal properties of the flame‐retardant PS were investigated by thermogravimetric analysis, limiting oxygen index (LOI), vertical burning test (UL‐94), scanning electronic microscopy, dynamic mechanical thermal analysis, and the real‐time Fourier transform infrared spectrometry (FTIR). The maximal decomposition rate temperature of PS/IFR containing Ce‐TNTs in air is much higher than that of other PS composite without Ce‐TNTs. The LOI value of PS/IFR that contained 0.1 wt% of Ce‐TNTs was increased from 27.0 to 28.5, and the UL‐94 rating was also enhanced to V‐0 from no rating when the total loading of additive was the same. The real‐time FTIR showed that the degradation process was changed after the addition of TNTs. All results indicated that Ce‐TNTs had a significant synergistic effect on the flame retardancy of PS/IFR. Copyright © 2012 John Wiley & Sons, Ltd.