海藻硫酸多糖抑制草酸钙结石形成的化学模拟

用体外模拟方法研究了从海藻异枝麒麟菜中提取的硫酸多糖(ESPS)对尿结石患者尿液中草酸钙晶体生长的影响. ESPS不但诱导与尿路细胞膜粘附力较弱的二水草酸钙晶体形成, 而且抑制一水草酸钙的生长和聚集, 归因于一水草酸钙的富钙(101)晶面与聚阴离子ESPS之间的静电相互作用. 上述结果表明, ESPS是一种抑制草酸钙结石的潜在绿色药物.     

茯苓菌丝体多糖的分离及结构分析

由茯苓菌种在培养基中于 2 5℃下培养一周得茯苓菌丝体 .分别用 0 9%NaCl水溶液、热水、0 5mol/LNaOH和 88%甲酸从该茯苓菌丝体中提取出四种多糖 ,编号为PCM1 ,PCM2 ,PCM3和PCM4 .用红外光谱 (IR) ,高效液相色谱 (HPLC) ,气相色谱 (GC)及13 C 核磁共振 ( 13 C NMR)等方法分析了它们的组成和结构 .结果表明 ,PCM1 ,PCM2为酸性杂多糖由D 鼠李糖、D 木糖、D 甘露糖、D 半乳糖、D 葡萄糖及葡萄糖醛酸组成 .PCM3主要为线型 β ( 1→ 3 ) D 葡聚糖 ,其产率占茯苓菌丝体总量的 55 8% .PCM4由D 葡萄糖和葡萄糖醛酸组成 .茯苓菌丝体化学组成和结构基本同于茯苓菌核多糖 ,随提取过程进行葡萄糖含量逐渐增加的变化规律也相同 .     

沙棘果JS1多糖结构研究中GC—MS及^13C—NMR分析

近年来由于新技术的发展和应用,糖类结构的测定和生物活性的研究取得了空前的进展,大量研究表明多糖具有多方面的生物活性,如增强机体的免疫能力、抗肿瘤和抗感染等,而且多数无毒副作用。     

海藻异枝麒麟菜多糖抑制尿石盐草酸钙晶体生长的研究

采用扫描电子显微镜(SEM)、 红外光谱(FTIR)和X射线衍射(XRD)方法研究了从海藻异枝麒麟菜中提取的硫酸多糖(ESPS)对草酸钙(CaOxa)晶体生长的影响. 结果表明, 添加ESPS能抑制一水草酸钙(COM)的生长, 同时诱导二水草酸钙(COD)晶体的形成. 随着ESPS的质量浓度从0增加到0.03和0.50 mg/mL, COD的质量分数从0分别增加到10%和55%; COM的(1 01)晶面加强, (020)晶面减弱直至消失, 并从三维晶体转变为棱角圆顿的四角形片状晶体; COM和COD的尺寸均明显变小. 这些结果表明, ESPS是抑制CaOxa结石形成的一种潜在药物.     

NMR对苯并噁嗪类化合物结构的研究

利用'H、'13CNMR谱及HMBC、HMQC二维谱对10种苯并噁嗪类化合物的结构进行了研究,初步得出了它们的NMR谱特征,分析了化学位移的影响因素。     

海藻酸钙多孔微球-白芨多糖复合止血粉的制备及止血性能评价

海藻酸盐具有良好的生物相容性、可降解性、止血、抗菌、促愈合等特性,而中药白芨中的白芨多糖具有收敛止血、消肿生肌的功效。用海藻酸盐和白芨多糖为原料,采用冷冻干燥技术制备海藻酸钙多孔微球-白芨多糖复合止血粉,对其吸水速率进行考核,并采用体外凝血和动物出血模型实验进行止血性能评价。结果表明,致孔剂的添加量为0.5%的海藻酸钙多孔微球,当其与白芨多糖的质量比1:1时制备的止血粉的止血效果最好。     

固定床渣油加氢脱金属废催化剂上焦炭结构和组成沿床层变化研究

针对取自中石油某装置不同床层轴向位置的工业固定床渣油加氢脱金属废催化剂,采用元素分析、热重分析、X射线光电子能谱、傅里叶变换红外光谱和核磁共振碳谱等,研究了催化剂上沉积焦炭的结构组成特征参数。结果表明,不同轴向位置废催化剂上的焦炭具有某些共同特征,如相同的碳类型和官能团等,但其结构和组成各不相同。模拟建立了基于各种表征结果的焦炭结构组成模型,并利用可计算核磁共振波谱化学位移和预测核磁共振谱图的gNMR软件对所建立焦炭模型的精确性进行了验证,表明模型与实验结果具有很好的一致性。     

碳-13核磁共振法研究小皮伞多糖结构

采用＾１３Ｃ核磁共振法测定和确定了小皮伞多糖中的大分子葡聚糖,葡甘聚糖等３种多糖的一级结构,这些结果与组成分析和甲基化分析结果是一致的,确定了毫克级直接用＾１３Ｃ核磁共振法分析和检测多糖结构的方法。     

海藻多糖中硫酸基含量对抑制草酸钙晶体形成和修复受损伤肾小管上皮细胞的影响

采用X射线衍射法、傅里叶变换红外光谱仪、扫描电子显微镜、ζ电位仪和电感耦合等离子体发射光谱仪,比较了4种分子量相近(约3 700 Da)、但硫酸基(—OSO₃^-)含量不同的降解海藻多糖对草酸钙(CaC₂O₄)晶体生长的调控作用;采用细胞实验比较了它们对受损伤肾小管上皮细胞(HK-2)的修复能力。这4种海藻多糖分别是降解紫菜多糖(PY-1)、降解龙须菜多糖(GL-2)、降解羊栖菜多糖(SF-3)和降解裙带菜多糖(UP-4),其—OSO₃^-含量分别为17.9%、13.3%、8.2%和5.5%。结果表明,这4种多糖均能够抑制一水草酸钙(COM)生长,诱导二水草酸钙(COD)生成,增加溶液中可溶性Ca²⁺离子浓度,增加晶体表面的ζ电位绝对值,从而降低晶体的聚集程度;这些多糖均能修复被草酸氧化损伤的HK-2细胞,提高细胞活力和超氧化物歧化酶(SOD)活力,降低丙二醛(MDA)的释放量。结果表明,多糖中—OSO₃^-...     

海藻多糖中硫酸基含量对抑制草酸钙晶体形成和修复受损伤肾小管上皮细胞的影响

采用X射线衍射法、傅里叶变换红外光谱仪、扫描电子显微镜、ζ电位仪和电感耦合等离子体发射光谱仪,比较了4种分子量相近(约 3 700 Da)、但硫酸基(—OSO₃^-)含量不同的降解海藻多糖对草酸钙(CaC₂O₄)晶体生长的调控作用;采用细胞实验比较了它们对受损伤肾小管上皮细胞(HK-2)的修复能力。这4种海藻多糖分别是降解紫菜多糖(PY-1)、降解龙须菜多糖(GL-2)、降解羊栖菜多糖(SF-3)和降解裙带菜多糖(UP-4),其—OSO₃^-含量分别为17.9%、13.3%、8.2%和5.5%。结果表明,这4种多糖均能够抑制一水草酸钙(COM)生长,诱导二水草酸钙(COD)生成,增加溶液中可溶性 Ca²⁺离子浓度,增加晶体表面的 ζ 电位绝对值,从而降低晶体的聚集程度;这些多糖均能修复被草酸氧化损伤的HK-2细胞,提高细胞活力和超氧化物歧化酶(SOD)活力,降低丙二醛(MDA)的释放量。结果表明,多糖中—OSO₃^-含量越高,多糖对 CaC₂O₄晶体生长的抑制作用和对受损伤 HK-2细胞的修复作用均越强。     

Isolation,Characterization, and Compositional Analysis of Polysaccharides from Pinot Noir Wines: An Exploratory Study

It has been reported that polysaccharides in wine can interact with tannins and other wine components and modify the sensory properties of the wine. Unfortunately, the contribution of polysaccharides to wine quality is poorly understood, mainly due to their complicated structure and varied composition. In addition, the composition and molecular structure of polysaccharides in different wines can vary greatly. In this study, the polysaccharides were isolated from pinot noir wine, then separated into high-molecular-weight (PNWP-H) and low-molecular-weight (PNWP-L) fractions using membrane-based ultrafiltration. Each polysaccharide fraction was further studied using size exclusion chromatography, UV–Vis, FT-IR, matrix-assisted laser desorption/ionization–high-resolution mass spectrometry, and gas chromatography-mass spectrometry (GC-MS). The results showed that PNWP-L and PNWP-H had different chemical properties and compositions. The FT-IR analysis showed that PNWPs were acidic polysaccharides with α- and β-type glycosidic linkages. PNWP-L and PNWP-H had different α- and β-type glycosidic linkage structures. FT-IR showed stronger antisymmetric and symmetric stretching vibrations of carboxylate anions of uronic acids in PNWP-L, suggesting more uronic acid in PNWP-L. The size exclusion chromatography results showed that over 72% of the PNWP-H fraction had molecular sizes from 25 kDa to 670 kDa. Only a small percentage of smaller molecular polysaccharides was found in the PNWP-H fraction. In comparison, all of the polysaccharides in the PNWP-L fraction were below 25 KDa, with a majority distributed approximately 6 kDa (95.1%). GC-MS sugar composition analysis showed that PNWP-L was mainly composed of galacturonic acid, rhamnose, galactose, and arabinose, while PNWP-H was mainly composed of mannose, arabinose, and galactose. The molecular size distribution and sugar composition analysis suggested that the PNWP-L primarily consisted of rhamnogalacturonans and polysaccharides rich in arabinose and galactose (PRAG). In comparison, PNWP-H were mostly mannoproteins and polysaccharides rich in arabinose and galactose (PRAG). Further research is needed to understand the impacts of these fractions on wine organoleptic properties.     

茯苓菌核多糖的分离和结构分析

分别用０．９％ＮａＣｌ不溶液，热水，０．５ｍｏｌ／Ｌ ＮａＯＨ水溶液和８８％甲酸从新鲜茯苓菌核体中提取出５种多糖：ＰＣ１，ＰＣ２，ＰＣ２－Ａ，ＰＣ３和ＰＣ４．用ＩＲ，ＨＰＬＣ，ＧＣ，＾１ＨＮＭＲ和＾１３Ｃ ＮＭＲ等方法分析了它们的组成和结构。结果表明，ＰＣ１，ＰＣ２和ＰＣ２－Ａ由Ｄ－葡萄糖，Ｄ－木糖，Ｄ－甘露糖和Ｄ－半乳糖组成，ＰＣ１和ＰＣ２－Ａ含葡萄糖醛酸，其葡萄糖含量随提取过程的进行逐渐增加。     

Morphology and Structure of Crystalline Polysaccharides: Some Recent Studies

Summary: In this paper, we review recent studies on the morphology and molecular structure of some polysaccharide crystals from amylose, cellulose, and mannan. The data were recorded using combinations of imaging, diffraction, and spectroscopic techniques: scanning and transmission electron microscopy, electron, neutron, and X-ray diffraction, as well as ¹³C solid-state NMR spectroscopy. Differences were generally found between native crystals, whose features result from in vivo biogenesis and the recrystallized products prepared in vitro.     

Microwave Assisted Graft Copolymerization of N-Isopropyl Acrylamide and Methyl Acrylate on Cellulose: Solid State NMR Analysis and CaCO3 Crystallization

Summary: Graft copolymerization of N-isopropyl acrylamide and methyl acrylate on α-cellulose was carried out under microwave irradiation at specific cut off temperatures with cerium (IV) ammonium nitrate and potassium persulfate (KPS) as the initiating system. The role of KPS was to oxidize Ce (III) to Ce (IV) which is the active species in radical formation. The reactions at a temperature cut off of 60 °C were confirmed by ¹³C nuclear magnetic resonance cross-polarization with magic- angle spinning (¹³C NMR CP/MAS) and Fourier-transform infrared spectroscopy (FTIR). The extent of grafting was calculated from weight gain and ¹³C resonances. The grafted cellulose was thermally more stable than the parent cellulose. An attempt to do grafting at a higher cut off temperature of 80 °C was made, however, no grafting was observed from ¹³C NMR CP/MAS but TGA results showed that a cellulose having more thermal stability resulted which was attributed to cross linking. Crystallization of CaCO₃ was carried out using the grafted materials as templates showed better nucleation and different crystal structure was observed.     

碱溶性茶多糖的提取及其分析

在煎煮后的低档绿茶茶渣中提取碱溶性茶多糖,经HPGPC-ELSD法分析其含有3种均一性多糖组分,依出峰顺序其质量分数约为5.96%、78.99%和15.05%;GC-MS法测得组成碱溶性茶多糖的6种单糖:鼠李糖、阿拉伯糖、木糖、甘露糖、葡萄糖和半乳糖,并分析了其摩尔比例.紫外-可见吸收光谱分析显示,碱溶性茶多糖在250～290 nm区段有"波浪状"吸收.红外光谱表征了碱溶性茶多糖的特征,圆二色谱分析了其水溶液的cotton效应.结果表明,在190 nm有正cotton效应,在203 nm有负cotton效应.     

乌龙茶多糖OTPS 2-1的光谱特性、形貌特征及热特性研究

采用纤维素和葡聚糖凝胶柱层析法分离纯化,获得乌龙茶多糖主要组分OTPS2-1.经GC,HPLC,UV,IR和GPC-LLS证实OTPS2-1是富含糖醛酸和少量蛋白质的三元糖复合物,相对重均分子量为8.877×10⁴,糖基由半乳糖、葡萄糖、阿拉伯糖、岩藻糖和鼠李糖组成,其摩尔比为7.58:2.14:7.05:1.76:1.02.利用AFM,QELS及LSCM观察OTPS2-1在溶液中的形貌特征,结果表明,OTSP2-1在溶液中呈直径0.2～0.5μm、高度0.3～0.6μm的短棒形不均一聚集体,并具有强烈的荧光,溶液的pH值显著影响其聚集行为.pH值、离子强度和络合物等环境因素的改变,均导致多糖立体构象和非对称性的变化.OTPS2-1在SEM低倍镜下呈折叠卷曲形貌,在高倍镜下呈现平整的图像.综合热分析结果表明,在加热过程中,多糖有3次大的质量损失过程,出现3次吸热峰和放热峰.提示茶叶经过半发酵处理后,多糖组成、分子质量分布以及分子间相互作用可引起微观形貌、链构象和聚集行为的变化,有利于提高生物活性.     

Click Chemistry with Polysaccharides

Summary: The copper‐catalyzed Huisgen reaction as a typical example of click chemistry was realized with the polysaccharide cellulose for the first time. The generality, selectivity, and the efficiency of click chemistry perfectly fit the requirements of polysaccharide modification, which is demonstrated by the introduction of triazole‐spacer bound functional groups, i.e., carboxylic ester, thiophene, and aniline moieties. Azide moieties introduced into cellulose via the tosyl derivative were simply transferred with ethynyl compounds under Cu(I) catalysis and mild and easily applicable conditions. Hydrolytically stable cellulose derivatives soluble in organic solvents, e.g., DMSO or DMF with DS up to 0.9 are obtained. The triazole substituted cellulose derivatives were characterized by elemental analysis, FTIR, ¹H NMR, and ¹³C NMR spectroscopies and show no impurities or substructures resulting from side reactions.

6‐Azido‐6‐deoxy cellulose.     

水溶性铑－膦配合物的结构及性能表征

采用ＩＣＰ、ＦＴＩＲ、１３ＣＷＲ、３１ＰＮＭＲ、ＴＧＡ、ＸＰＳ等方法，对三种水溶性铑配合物：ＨＲｈ（ＣＯ）（ＴＰＰＴＳ）３、ＲｈＣｌ（ＣＯ）（ＴＰＰＴＳ）２和ＲｈＩ（ＣＯ）（ＴＰＰＴＳ）２的组成、结构和性质进行了表征．结果表明，采用新设计的方法合成的水溶性铑－膦配合物，具有以三苯基膦为配体的配合物类似的结构．它们的热稳定性很好，在水中的溶解度大，而在非极性有机溶剂中极难溶解，是良好的烯烃氢甲酰化催化剂．     

Probing Helical Hydrophobic Binding Sites in Branched Starch Polysaccharides Using NMR Spectroscopy

Branched starch polysaccharides are capable of binding multiple hydrophobic guests, but their exploitation as multivalent hosts and in functional materials is limited by their structural complexity and diversity. Linear α(1–4)‐linked glucose oligosaccharides are known to bind hydrophobic guests inside left‐handed single helices in solution and the solid state. Here, we describe the development of an amphiphilic probe that binds to linear α(1–4)‐linked glucose oligosaccharides and undergoes a conformational switch upon complexation, which gives rise to dramatic changes in the ¹H NMR spectrum of the probe. We use this probe to explore hydrophobic binding sites in the branched starch polysaccharides amylopectin and β‐limit dextrin. Diffusion‐ordered (DOSY), nuclear Overhauser effect (NOESY) and chemical shift perturbation (HSQC) NMR experiments are utilised to provide evidence that, in aqueous solution, branched polysaccharides bind hydrophobic guests in well‐defined helical binding sites, similar to those reported for complexation by linear oligosaccharides. By examining the binding affinity of the probe to systematically enzymatically degraded polysaccharides, we deduce that the binding sites for hydrophobic guests can be located on internal as well as external branches and that proximal α(1–6)‐linked branch points weaken but do not prevent complexation.     

Binding and Removal of Aluminum Ions in Waters by an Algal Biomass

Abstract

A preliminary study on the binding and removal of trace concentrations of aluminum ions in waters by two species of algae, Chlorella Pyrenoidosa and Chlorella Vulgaaris, were investigated. Binding by the former was minimal over all pH ranges, but binding by the latter was effective with a maximum binding of 68% occurring at pH 5. Binding was lowered drastically below pH 2, and this may be used to remove aluminum from the algae. Optimum binding occurred after 20 minutes exposure time of algae to aluminum solution and 450 mg algae mass to 100 mL solution. Binding was reproducible and more efficient in waters with low suspended solids. High salt concentrations interfere with binding, and the Chlorella Vulgaris could be reused 7 times with washings between each binding before a noticeable decrease in binding efficiency was found.