新型可溶性酞菁铜(Ⅱ)衍生物的合成、结构及其成膜性

合成了两个新型取代酞菁铜(Ⅱ)衍生物:四-4-(2-甲氧基乙氧基-羰基)酞菁铜(Ⅱ)(A)和四-4-(2-正丁氧基乙氧基-羰基)酞菁铜(Ⅱ)(B),以元素分析、ESR、~1H NMR和FT-IR进行了表征。UV-vis光谱表明它们在氯仿溶液(10~(-5)～10(-6)mol/L)中主要以双分子缔合形式存在;X-射线粉末衍射表明配合物的分子以倾斜的方式相互平行排列;热重分析表明酞菁环引入有机基团后其热稳定性略有下降,且取代基越长,热稳定性越差。两个配合物的氯仿溶液在亚相(水)上的π-A曲线表明,它们均有明显的“气”液”“固”的变化过程,并能形成较好的单分子层膜。

两种新型抗癌药的结构鉴定

本文应用质谱、核磁共振波谱、红外光谱及元素分析等方法对1-(2-四氢呋喃)-5-氟脲嘧啶(FT-207)和1,3-双(2-四氢呋喃)-5-氟脲嘧啶(FD-1)两种新型抗癌药进行了结构鉴定。

液体多脉冲及二维FT—NMR实验的乘积算符描述的计算机模拟

本文报道了利用乘积算符方法分析多脉冲及二维FT-NMR实验的模拟程序PROPER-MT.该程序对分析弱耦合I_mS_n(I=1/2;S=1/2;1≤m十n<4)自旋体系实验脉冲序列是普遍适用的;它可给出实验过程中体系任何时刻算符的解析表达式.用PROPER-MT程序对一些典型的多脉冲及二维FT-NMR实验进行了模拟,特别对多量子滤波及多自旋滤波脉冲序列进行了分析计算,得到了预期的结果.

稀土HEH[EHP]固体配合物的红外光谱

本文制备了La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu,Y等十五种稀土与2-乙基己基膦酸单(2-乙基己基)酯的固体配合物,测定了4000-100cm~(-1)的FT-IR光谱,对其主要红外光谱吸收带进行了归属。指认150cm~(-1)为Ln-O键的伸缩振动带,250cm~(-1)附近的谱带为COPO,CCPO骨架扭曲振动与Ln-O键的耦合振动带。结果表明配合物为多聚体系,PO_2与稀土离子可能为桥式配位形式。Ln-O键基本上为离子键。

聚苯乙烯-乙丙共聚物两嵌段共聚物的组成分析

本文用红外光谱(IR)的工作曲线法及傅里叶变换红外光谱(FT-IR)差谱法,分析了多单体嵌段共聚物聚苯乙烯-乙丙共聚物PS-b-EPR的组成,包括聚苯乙烯段的含量和乙丙共聚物段的乙丙组成。

The preparation and bioactivity research of agaro-oligosaccharides

Agaro-oligosaccharides were hydrolytically obtained from agar using hydrochloric acid, citric acid, and cationic exchange resin (solid acid). The FT-IR and NMR data showed that the hydrolysate has the structure of agaro-oligomers. Orthogonal matrix method was applied to optimize the preparation conditions based on alpha-naphthylamine end-labeled HPLC analysis method. The optimal way for oligosaccharides with different degree of polymerization (DP) was achieved by using solid acid degradation, which could give high yield and avoid solution neutralization process. Agaro-oligosaccharides with high purity were consequently obtained by activated carbon column isolation. Furthermore, the antioxidant and alpha-glucosidase inhibitory activity of three fractions were also investigated. The result indicated that 8% ethanol-eluted fraction showed highest activity against alpha-glucosidase with IC50 of 8.84 mg/mL, while 25% ethanol-eluted fraction possessed excellent antioxidant ability.

水处理纳米材料的制备、性能及应用研究

工业的高速发展使地球上有限的水资源受到日益严重的污染，去除水中的有毒、有害化学物质已成为环保领域的一项重要工作。纳米材料与技术的开发应用为实现高效、低成本的水处理开辟了新的途径。 本课题组开发的纳米-亚纳米功能新材料（生态宝）可用作养殖生态环境改良剂，它对“三氮”、硫化物、CODCr、BOD5、重金属等有害物质具有很好的去除能力。生态宝用于养殖幼参，有显著的促生长、增加成活率的作用。生态宝用于养殖对虾，对虾体内重金属含量有明显降低。 以粉末状P25型纳米TiO2为光催化剂，系统的研究了它对染料AB80的光催化降解。在紫外光照射下，光催化反应75min，染料AB80溶液完全脱色，光催化反应135min，染料溶液完全矿化；AB80的光催化脱色反应遵从准一级反应动力学；催化剂的最佳剂量为1.0g/L。AB80在TiO2颗粒表面的吸附符合Langmuir方程式，随着pH值的增加吸附量迅速减少；pH值在反应中起着重要的作用，碱性溶液中的反应速度比酸性溶液的大，pH=10.0初始反应速度最大；电子捕获剂（H2O2）的加入能够显著的提高反应速率，H2O2浓度为5mmol/L时，反应速度变为原来的2.78倍。 以硅藻土为载体，采用溶胶-凝胶法制备了负载型的纳米TiO2，SEM分析结果表明，TiO2的包覆量对负载光催化剂的形貌有很大影响，TiO2包覆量较低(14.5%)的复合物无团聚现象发生。XRD分析结果表明，所制备的TiO2为锐钛矿和金红石混晶型，平均粒径11nm。FT-IR分析结果表明，TiO2和硅藻土之间没有生成化学键。以染料AB80和B-2BF为模型污染物，利用制备的光催化剂复合物进行了吸附-光催化试验，结果表明，TiO2包覆量为14.5%的复合物具有较高的吸附-光催化活性，对模型污染物的降解效果好于德国Degussa公司的商品纳米P25-TiO2。溶液pH对TiO2/硅藻土复合物光催化活性影响很大，弱酸性条件有利于反应的进行。TiO2/硅藻土对实际印染废水有较好的降解效果，试验条件下，废水光催化反应3.5h，色度去除率为100%。研究了液固多相光催化反应的催化剂失活原因及再生手段，提出TiO2/硅藻土复合物再生的方法为酸洗和高温烧结。对于模拟印染废水来说，光催化剂重复使用对光催化活性几乎没有影响，重复使用15次后，催化活性仅降低了12%。而对实际印染废水来说，重复使用对光催化活性有影响，光催化剂复合物重复使用7次后，催化活性降低了41%。TiO2/硅藻土复合光催化剂成本低，简便易行，光催化效果好，有望在环境污染物治理中得到广泛的应用。 采用CuCl水解法制得了硅藻土负载的纳米Cu2O，并利用XRD、SEM等手段对其进行表征。研究了负载的纳米Cu2O对B-2BF和AB80染料废水的光催化降解，发现纳米Cu2O经过负载后，团聚减少，分散性好，对染料废水的光催化降解效率成倍增长。纳米Cu2O包覆量为31.3%的光催化剂复合物光催化活性最好，其光催化效率是纯的Cu2O的6倍。负载的纳米Cu2O可以有效的利用太阳光进行光催化反应，而且太阳光下纳米Cu2O的光催化活性比纳米TiO2的强。太阳能是取之不尽、用之不竭的清洁能源，利用太阳能来处理染料废水成本低、无污染，是一种非常有发展前景的环境治理新技术。pH 5-pH 7是负载纳米Cu2O光催化降解B-2BF的最佳反应范围。负载的纳米Cu2O光催化剂有较好的稳定性，重复使用8次以后，其脱色率仍能达到75%以上。

In vitro antioxidant activities of acetylated, phosphorylated and benzoylated derivatives of porphyran extracted from Porphyra haitanensis

Porphyran extracted from red algae Porphyra haitanensis is a sulfated polysaccharide, which possesses excellent antioxidant activities. In this study, we prepared the acetylated, phosphorylated and benzoylated derivatives of porphyran. And then the antioxidant activities of all the samples were investigated including scavenging effects of superoxide and hydroxyl radicals and reducing power. The results of chemical analysis and FT-IR spectrum showed the modifications of porphyran were successful. And in addition, we found that certain derivative exhibited stronger antioxidant activity than raw material. And the mechanism of the structure-function relationship of these derivatives needs to be attended to. (C) 2009 Elsevier Ltd. All rights reserved.

Preparation of the different derivatives of the low-molecular-weight porphyran from Porphyra haitanensis and their antioxidant activities in vitro

Porphyran extracted from Porphyra haitanensis is a sulfated polysaccharide, which possesses excellent antioxidant activities. In this study, we prepared one low-molecular-weight porphyran and its sulfated, acetylated, phosphorylated and benzoylated derivatives. Their antioxidant activities were investigated including scavenging effect of superoxide, hydroxyl and 1,1-diphenyl-2-picrylhydrazyl radicals. The results of chemical analysis and FT-IR spectrums showed the modification was successful. And in addition, we found that certain derivative exhibited stronger antioxidant activity than low-molecular-weight porphyran. The benzoylated derivative showed the most excellent antioxidant activity in three assays, so this derivative needs to be attended to. (C) 2009 Elsevier B.V. All rights reserved.

Antimicrobial activity of hydroxylbenzenesulfonailides derivatives of chitosan, chitosan sulfates and carboxymethyl chitosan

Chitosan, carboxymethyl chitosan (CIVICS) and chitosan sulfates (CSS) with different molecular weight were modified by reacting with 4-hydroxyl-5-chloride-1,3-benzene-disulfo-chloride or 2-hydroxyl-5-chloride-1,3 -benzene-disulfo-chloride to give 12 kinds of new hydroxylbenzenesulfonailides derivatives of them. The preparation conditions of the derivatives were discussed in this paper, and their structures were characterized by FT-IR and C-13 NMR spectroscopy. The solubility of the derivatives was measured in the experiment. In addition, their antimicrobial activities against four bacteria and five crop-threatening pathogenic fungi were tested in the experiment. Besides, the rule and mechanism of their antibacterial activities were discussed in this paper. (C) 2009 Published by Elsevier B.V.

Preparation, characterization and antifungal properties of 2-(alpha-arylamino phosphonate)-chitosan

In this paper, 20 kinds of different 2-(alpha-arylamino phosphonate)-chitosan (2-alpha-AAPCS) were prepared by different Schiff bases of chitosan (CS) reacted with di-alkyl phosphite in benzene solution. The structures of the derivatives (2-alpha-AAPCS) were characterized by FT-IR spectroscopy and elemental analysis. In addition, the antifungal activities of the derivatives against four kinds of fungi were evaluated in the experiment. The results indicated that all the prepared 2-alpha-AAPCS had a significant inhibiting effect on the investigated fungi when the derivatives concentration ranged from 50 to 500 mu g mL(-1). Furthermore, the antifungal activities of the derivatives increased with increasing the molecular weight and concentration. And the antifungal activities of the derivatives were affected by their dimensional effect and charge density. Besides, the rule and mechanism of the antifungal activities of them were discussed in this paper. (C) 2009 Elsevier B.V. All rights reserved.

Polysaccharides from Ulva pertusa (Chlorophyta) and preliminary studies on their antihyperlipidemia activity

Polysaccharides from Ulva pertusa were isolated and prepared by extraction in hot water and precipitation by ethanol. The water-soluble polysaccharides were chemically well defined, containing 47.0% total carbohydrate, 23.2% uronic acids, 17.1% sulfate groups, 1.0% N and 29.9% ash. Gas chromatography analysis demonstrated that the neutral sugars were mainly composed of rhamnose, xylose and glucose and smaller amounts of mannose, galactose and arabinose. The FTIR and C-13-NMR spectra indicated that basic repeating units of the polysaccharides were (beta-D-GlcpA-(1->4)-alpha-L-Rhap 3S) and (alpha-L-IdopA-(1->4)-alpha-L-Rhap 3S). Fifty ICR mice were used to study the effect of water-soluble polysaccharides from Ulva pertusa on the level of plasma lipids, with inositol niacinate as positive control. The results indicated that the polysaccharides significantly lowered the contents of plasma total cholesterol, low-density lipoprotein cholesterol, triglyceride and markedly increased the contents of serum high-density lipoprotein cholesterol, compared with the hyperlipidemia control group (p<0.01). Moreover, administration of polysaccharides significantly decreased the atherogenic index. The present results suggest that the polysaccharides from Ulva pertusa have great potential for preventing ischemic cardiovascular and cerebrovascular diseases.

Synthesis and antifungal properties of sulfanilamide derivatives of chitosan

Sulfanilamide derivatives of chitosan (2-(4-acetamido-2-sulfanimide)-chitosan (HSACS, LSACS), 2-(4-acetamido-2-sulfanimide)-6-sulfo-chitosan (HSACSS, LSACSS) and 2-(4-acetamido-2-sulfanimide)-6-carboxymethyl-chitosan (HSACMCS, LSACMCS)) were prepared using different molecular weights of chitosan (CS), carboxymethyl chitosan (CMCS) and chitosan sulfates (CSS) reacted with 4-acetamidobenzene sulfonyl chloride in dimethylsulfoxide solution. The structures of the derivatives were characterized by FT-IR spectroscopy and elemental analysis, which showed that the substitution degree of sulfanilamide group of HSACS, HSACSS, HSACMCS, LSACS, LSACSS and LSACMCS were 0.623, 0.492, 0.515, 0.576, 0.463 and 0.477, respectively. The solubility of the derivatives (pH < 7.5) was higher than that of chitosan (pH < 6.5). The antifungal activities of the derivatives against Aiternaria solani and Phomopsis asparagi were evaluated based on the method of Jasso et al. in the experiment. The results indicated that all the prepared sulfanilamide derivatives had a significant inhibiting effect on the investigated fungi in the polymer concentration range from 50 to 500 mu g mL(-1). The antifungal activities of the derivatives increased with increasing the molecular weight, concentration or the substitution degree. The sulfanilamide derivatives of CS, CMCS and CSS show stronger antifungal activities than CS, CMCS and CSS. (C) 2007 Elsevier Ltd. All rights reserved.

Synthesis of acyl thiourea derivatives of chitosan and their antimicrobial activities in vitro

Three different acyl thiourea derivatives of chitosan (CS) were synthesized and their structures were characterized by FT-IR spectroscopy and elemental analysis. The antimicrobial behaviors of CS and its derivatives against four species of bacteria (Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, and Sarcina) and four crop-threatening pathogenic fungi (Alternaria solani, Fusarium oxysporum f. sp. vasinfectum, Colletotrichum gloeosporioides (Penz.) Saec, and Phyllisticta zingiberi) were investigated. The results indicated that the antimicrobial activities of the acyl thiourea derivatives are much better than that of the parent CS. The minimum value of MIC and MBC of the derivatives against E coli was 15.62 and 62.49 mu g/mL, respectively. All of the acyl thiourea derivatives had a significant inhibitory effect on the fungi in concentrations of 50 - 500 mu g/mL; the maximum inhibitory index was 66.67%. The antifungal activities of the chloracetyl thiourea derivatives of CS are noticeably higher than the acetyl and benzoyl thiourea derivatives. The degree of grafting of the acyl thiourea group in the derivatives was related to antifungal activity; higher substitution resulted in stronger antifungal activity. (c) 2007 Elsevier Ltd. All rights reserved.

The antioxidant activity of 2-(4(or 2)-hydroxyl-5-chloride-1,3-benzene-di-sulfanimide)-chitosan

Chitosan (CS) with two different molecular weights was modified by reacting with 4-hydroxyl-5-chloride-1,3-benzene-disulfo-chloride or 2-hydroxyl-5-chloride-1,3-benzene-disulfo-chloride to give new 2-(4(or 2)-hydroxyl-5-chloride-1,3-benzene-di-sulfanimide)-chitosan (2-HCBSAHCS, 2-HCBSALCS, 4-HCBSAHCS, 4-HCBSALCS). The structure of the derivatives was characterized by FT-IR and C-13 NMR spectroscopy. The antioxidant activities of the derivatives were investigated employing various established systems, such as hydroxyl radical ((OH)-O-center dot)/superoxide anion (O-2(radical anion)) scavenging/reducing power and chelating activity. All the derivatives showed stronger scavenging activity on hydroxyl radical than chitosan and ascorbic acid (Vc), and IC50 of 4-HCBSAHCS, 4-HCBSALCS, 2-HCBSAHCS and 2-HCBSALCS was 0.334, 0.302, 0.442, 0.346 mg/mL, respectively. The inhibitory activities of the derivatives toward superoxide radical by the PMS-NADH system were strong. The results showed that the superoxide radical scavenging effect of 2-(4(or 2)-hydroxyl-5-chloride-1,3-benzene-disulfanimide)-chitosan was higher than chitosan. The derivatives had obviously reducing power and slight chelating activity. The data obtained in in vitro models clearly establish the antioxidant potency of 2-(4(or 2)-hydroxyl-5-chloride-1,3-benzene-disulfanimide)-chitosan. (C) 2007 Elsevier Masson SAS. All rights reserved.