几种海藻多糖硫酸酯碱式铝盐的制备

本文以褐藻胶和κ-卡拉胶为原料通过酸水解分别获得了低聚的甘露糖醛酸、古罗糖醛酸和低聚 κ-卡拉胶 ,并采用 HPGPC法测定了这 3种低聚糖的重均分子量。在此基础上再经硫酸酯化和成盐修饰制备了各自的硫酸酯碱式铝盐。对制得的几种碱式铝盐进行了红外光谱 (IR)分析和有机硫含量 (S% )、铝含量 (Al% )及样品制酸力等部分理化性质的测定。测定结果初步显示出这几种海藻多糖硫酸酯碱式铝盐较好的抗消化性溃疡前景。     

应用硫酸苯酚法建立一种甘露糖醛酸C-5差向异构酶活性检测方法的研究

建立了一种简便快捷的甘露糖醛酸C-5差向异构酶活性的测定方法。研究发现相同分子质量的聚甘露糖醛酸和聚古罗糖醛酸与苯酚硫酸试剂反应后显色程度不同,以此可以用来测定β-D-甘露糖醛酸/α-L-古罗糖醛酸(M/G)值的变化,从而计算甘露糖醛酸C-5差向异构酶的活性。利用本方法测定了已知结构的褐藻胶片断的M/G比,其结果与传统的1H-NMR测定值基本一致。     

不饱和古罗糖醛酸三糖和甘露糖醛酸三糖的结构表征

以双功能褐藻胶裂解酶 (Pseudoalteromonas sp.strain No. 2 72 )分别降解均聚古罗糖醛酸(PG)和均聚甘露糖醛酸 (PM) ,经 Bio- Gel- P6和 POROS- HQ2 0分离得到 2种三糖纯品 ,经 ESI- MS,1 H- NMR,1 3 C- NMR,1 H- 1 H COSY,1 H- 1 3 C HMQC确定其结构为 Δ4,5-古罗糖醛酸 - α(1→ 4 ) - L-古罗糖醛酸 -α(1→ 4 ) - L -古罗糖醛酸 (简写为Δ GG)和Δ4,5-甘露糖醛酸 -β (1→ 4 ) - D-甘露糖醛酸 -β (1→ 4 ) - D-甘露糖醛酸 (ΔMM) ,为进一步从事构效关系研究提供结构信息。     

两种不同凝胶柱测定壳聚糖分子量结果的比较

凝胶渗透色谱法测定壳聚糖分子量 ,以葡聚糖为标准品 ,用 2种不同的凝胶柱 (PLaquagel- OH柱和 TSK G4 0 0 0 PWXL柱 )测定 4种样品的分子量及其分布 ,并经过普适标定。比较结果发现 :PL aquagel- OH柱效果稍好于 TSK G4 0 0 0 PWXL柱。两柱所得重均分子量平均偏差为 0 .17%～ 3.38% ,数均分子量的平均偏差为 0 .90 %～ 3.5 7% ,分子量分布宽度指数 1.34～ 1.5 4。     

褐藻酸中糖醛酸组分的测定

褐藻胶于1883年首次由英国化学家Stanford从掌状海带(Laminaria digitata)加碱提取得到的。1929年,Nelson等证实褐藻胶的组成单位为D-甘露糖醛酸。从此,人们一直认为D-甘露糖醛酸是褐藻酸的唯一组分。1955年,Fischer等用纸层析法首次确定褐藻酸中除D-甘露糖醛酸外,尚含有L-古罗糖醛酸和少量葡萄糖醛酸。其后Whistler等以及Hirst等相继证实了褐藻胶中确实有L-古罗糖醛酸存在。     

海洋硫酸多糖916在2种酶作用下稳定性的研究

利用高效凝胶渗透色谱法(HPGPC)和明胶比浊法研究了海洋硫酸多糖916在溶菌酶和胰蛋白酶作用下的稳定性，分别考察了酶作用下916的重均分子量、分子量分布系数和游离硫酸根含量的变化。结果表明：在所选定的实验条件下，916的重均分子量、分子量分布系数和游离硫酸根含量均未发生显著变化，表明在所选择的实验条件下916对溶菌酶和胰蛋白酶是稳定的。     

不同分子量海蚌类肝素理化性质分析及抗血栓活性评价

为探究不同分子量海蚌类肝素的理化性质、体内抗血栓活性及对出血时间的影响,本文以海蚌类肝素G2(60.25kDa)及其2种不同分子量的降解产物DG1(24.48kDa)、DG2(6.75kDa)为研究对象,首先采用改良的硫酸-咔唑法和BaCl₂-gel比浊法测定糖醛酸及硫酸基的含量,利用纳米粒径仪测定粒径、Zeta电位,并同步利用热分析仪分析热稳定性;然后通过小鼠黑尾模型和小鼠断尾模型分别研究抗血栓活性及对出血时间的影响。研究结果表明,随着分子量的降低,海蚌类肝素硫酸基含量升高,糖醛酸含量降低,初始降解温度先升高后降低,粒径降低, Zeta电位升高。相对于海蚌类肝素G2,其适度降解产物DG1具有更高的抑制尾部血栓形成的能力,同时具有较低的出血风险。     

富含古罗糖醛酸的褐藻多糖生产菌株的构建

为获得古罗糖醛酸(Guluronate)含量高的细菌胞外褐藻多糖,利用PCR从海洋细菌Pseudomonassp.QDA中克隆了其甘露糖醛酸C-5差向异构酶基因(algG),连接入质粒pMF 54Km,构建了重组表达载体pMF54 Km-algG。利用三亲接合法将pMF54 Km-algG转入菌株QDA中,获得algG过量表达重组菌株QDA-G1。H-NMR测定结果表明,QDA-G所产的褐藻多糖中β-D-甘露糖醛酸(M)与它的C-5差向异构体α-L-古罗糖醛酸(G)的比值为0.38,G的质量分数达到74.2%,比野生菌株QDA提高了26.4%。且重组菌株遗传稳定性良好,连续传代20代后,M/G的比值无明显变化。     

红树林海洋细菌PLM4抑制肿瘤细胞生长活性多糖的纯化及结构分析

红树林海洋短小芽孢杆菌Bacillus pumilus（PLM4）的发酵液对人喉癌细胞Hep-2、肝癌细胞BEL-7404和舌癌细胞TCA8123的生长抑制活性分别为63．6％、59．2％和61．5％。PLM4发酵液经乙醇沉淀和凝胶柱层析纯化可得到多糖纯品。采用高效凝胶渗透色谱法测定其分子量和纯度,硫酸-咔唑法、2,4-二硝基苯肼比色法、氯化钡明胶比色法、茚三酮反应和气相色谱法等测定其组分。采用红外光谱分析、高碘酸氧化和Smith降解等方法研究其结构。结果表明,该多糖分子量为116kd,由己糖醛酸、甘露糖、葡萄糖和丙酮酸组成,其摩尔比为31：19：6：1,不含硫酸、乙酸和蛋白质。平均每100个己糖基中含有约42个1→3糖苷键、42个1→6糖苷键和／或非还原末端基、13．5个1→2糖苷键和2．5个1→4糖苷键。     

几丁糖酯原料药稳定性研究

该文建立高效凝胶渗透色谱法 (HPGPC) ,明胶比浊法 ,氧瓶燃烧法三种分析方法考察海洋硫酸多糖药物几丁糖酯的稳定性 ,采用这三种方法分别考察几丁糖酯原料药在高温、高湿、强光照射及加速条件下分子量及分布宽度、样品中硫酸根含量及样品含量的变化情况。结果表明 :三种方法均适用于几丁糖酯的稳定性考察 ,几丁糖酯在上述影响因素条件下稳定性良好     

海萝藻(Gloiopeltis furcata)多糖的提取分离及其结构表征

以海萝藻(Gloiopeltis furcata)为原料,依次经冷水、热水和热碱溶液提取,从中获得了3种多糖(GFW,GFH和GFA),其得率分别为57.9%,2.5%和2.6%。运用气相色谱法(GC)、高效凝胶渗透色谱法(HPGPC)、红外光谱(IR)及核磁共振碳谱(13C-NMR)等方法对其单糖组成、分子量以及结构进行了分析。结果表明,GFW和GFH都只含有D-半乳糖(Gal)和3,6-内醚-L-半乳糖(AnG),而GFA除了含有Gal和AnG外,还有木糖;3种多糖的分子量分别为22.6 kD,26.5 kD和49.8 kD;硫酸基含量分别为31.2%,25.1%,22.7%。IR和13C-NMR数据均表明其硫酸基在半乳糖残基C6位。结论:海萝藻中多糖均为硫酸多糖,其中2种为硫琼胶,另一种为含有木糖的硫酸半乳聚糖。     

Methods to quantify components of the excavating sponge Cliona orientalis Thiele, 1900

This study applied the loss after combustion (LAC) method and the acid decalcification (ADC) method to quantify different components of an excavating sponge. Samples of dried coral skeleton of Favia sp. invaded by the Indo‐Pacific excavating sponge Cliona orientalis Thiele, 1900 were used. The sponge tissue penetrated the 12‐mm‐thick samples to approximately 10 mm. The average proportional weight of organic matter, siliceous spicules, calcareous substrate and salts in the entire samples was found to be respectively 2.5%, 4.4%, 90.5% and 2.5% of dry weight applying the LAC method, and 2.9%, 5.9%, 89.0% and 2.3% of dry weight applying the ADC method. Respective volumetric proportions of the organic matter, spicules, substrate and salts were then calculated to be 6.4%, 5.5%, 85.2% and 3.0% of volume with the LAC method, and 7.4%, 7.2%, 82.7% and 2.7% of volume with the ADC method. The LAC method showed low variability of data and is simple and fast and therefore is recommended. The ADC method generated very similar results to the LAC method. However, due to the handling involved in the ADC method, more than half of the spicules may be lost and the method is therefore not recommended unless careful data corrections are considered. In addition, the buoyant weight method was used to quantify actual substrate weight in the fresh sponge‐substrate samples. This method was found to be at least 97% effective, revealing that buoyant weights can potentially be used to quantify bioerosion rates of excavating sponges. To our knowledge, this is the first study to systemically quantify organic and inorganic components of an excavating sponge and its calcareous substrate, providing improved standard methods for future studies.     

控释海水植物肥中氮、磷的测定

为评价控释肥的肥效，探讨、建立了相应的氮、磷测定方法。用硫酸作消解剂，消解液可以同时被用来测定氮、磷。钼锑抗坏血酸络合物作为显色剂，用紫外可见分光光度计测定磷的浓度；用改良式微量凯氏定氮蒸馏滴定法测定氮的含量。该方法灵敏、准确，易操作。用海水浸泡自制的控释海水植物肥样品(编号：MRF-0201．中速型)，运用建立的氮、磷测定方法测定浸取液中的氮、磷含量，实验证明该方法可以用于研究控释海水植物肥在海水中的氮、磷的化学动力学行为。     

厚叶切氏海带多糖的提取分离及其结构表征

本文以厚叶切氏海带(Kjellmaniella crassifolia)为原料,经提取分离获得4种多糖(KW1,KW2,KA1和KA2)。运用电泳、高效液相色谱(HPLC)、高效凝胶渗透色谱(HPGPC)及核磁共振氢谱(1H-NMR)法分别对其单糖组成、相对分子量(Mr)以及结构进行分析。结果表明,KW1与KA1是Mr为520 kD和430 kD且M/G(6.14和1.90)显著不同的褐藻胶;KW2是以岩藻糖(82%)为主的岩藻糖硫酸酯;KA2是以半乳糖(34%)、岩藻糖(27%)和甘露糖(21%)为主的杂聚硫酸多糖。KW2和KA2的Mr和硫酸基含量分别为536 kD和427 kD及30%和21%。经1H-NMR分析表明,KW2的硫酸酯基主要存在于岩藻糖残基的C2和C4位。     

高压密闭消解-电感耦合等离子体光谱和质谱联合测定海洋地质样品中52种元素

An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method(HPCD), is studied by an inductively coupled plasma optical emission spectrometry(ICP-OES) and an inductively coupled plasma mass spectrometry(ICP-MS). The operating parameters of the instruments are optimized, and the optimal analytical parameters are determined. The influences of optical spectrum and mass spectrum interferences, digestion methods and acid systems on the analytical results are investigated. The optimal spectral lines and isotopes are chosen, and internal standard element of rhodium is selected to compensate for matrix effects and analytical signals drifting. Compared with the methods of an electric heating plate digestion and a microwave digestion, a high-pressure closed digestion method is optimized with less acid, complete digestion,less damage for digestion process. The marine geological samples are dissolved completely by a HF-HCl-HNO_3 system, the relative error(RE) for the analytical results are all less than 6.0%. The method detection limits are 2–40μg/g by the ICP-OES, and 6–80 ng/g by ICP-MS. The methods are used to determine the marine sediment reference materials(GBW07309, GBW07311, GBW07313), rock reference materials(GBW07103, GBW07104,GBW07105), and cobalt-rich crust reference materials(GBW07337, GBW07338, GBW07339), the obtained analytical results are in agreement with the certified values, and both of the relative standard deviation(RSD) and the relative error(RE) are less than 6.0%. The analytical method meets the requirements for determining 52 elements contents of bulk marine geological samples.     

羊栖菜不同分子质量褐藻多酚抗氧化活性研究

将羊栖菜(Sargassum fusiforme)经浸提、萃取和超滤等步骤获得不同分子质量的褐藻多酚。用普鲁士蓝法检测其总抗氧化能力;采用 DPPH、羟自由基试剂盒、超氧阴离子试剂盒评价其对 DPPH、羟自由基和超氧阴离子的清除能力。结果显示,羊栖菜褐藻多酚主要以高分子质量的形式存在;乙酸乙酯相组分各项抗氧化指标均好于水相,且乙酸乙酯相分子质量大于30000组分对羟自由基与超氧阴离子的清除能力比没食子酸、Vc和VE强。     

The stabilisation of wet sediment cores by means of a polyethylene glycol/freeze-drying treatment for display and permanent storage

A reversible method is presented to transform waterlogged sediment cores into dry and stable specimens which can go on exhibition or into permanent storage, needing no special precautions. Wet sediment core segments are bath-impregnated with polyethylene glycol of molecular weight 3,350 (PEG 3,350) dissolved in water. The samples are then subjected to a freeze-drying process, during which the PEG forms a stabilising and bonding porous network structure in the capillary system of the sediment. Standard sediment cores at least 1 m long become strong enough to stand upright. Sediment types ranging from muddy deep-sea sediments to very coarse littoral Halimeda sand were successfully stabilised. For standard cores of 10-cm diameters split length-wise, impregnation times vary from 2 weeks for coarse sand to 6–10 weeks for more compacted sediments. With regard to the stability of the samples and the visual clarity of detail, best results were obtained by impregnation with 25 to 60% solutions of PEG 3,350, coarse sediments needing more PEG than finer ones. Colour changes are systematic – the processed samples are lighter in appearance and the contrasts are enhanced, but there is no serious shift in colour tones. The PEG can easily be re-dissolved and washed out of the sediments. Display specimens can thus be made available for research again.     

The occurrence of high molecular weight humic material in recent organic-rich sediment from the Namibian shelf

The molecular size distribution of humic substances has been investigated in two recent sediment samples of different ages taken from a single core sample collected off Walvis Bay, south-west Africa. Extractable humic acids were found to be by far the major form of organic carbon in both sediments, the near-surface younger sample containing predominantly high molecular weight (>100 000 molecular weight) humic acids and little fulvic acids whilst the deeper, older sample contained relatively less humic acid and relatively more fulvic acid of a range of molecular weights. A significant age difference was found between the >300 000 molecular weight and the <30 000 molecular weight fractions of the near-surface sample, the lower molecular weight fraction being older than the higher molecular weight fraction.The data suggest that in this rapidly accumulating, organic-rich sediment the first step en route from the planktonic matter to the humic complexes is direct and rapid incorporation of the biogenic material into high molecular weight humic acids.     

海岛地区小康社会建设评价指标体系研究

文章以5个海岛县(区)为样本,采用分层次和多维度的综合评价方法,从经济持续健康发展、人民民主、文化软实力、人民生活水平和"两型"社会建设5个方面,选取人均GDP、网上参政度、初中毕业升高中率、人均社区财政支出和森林覆盖率等25个评价指标,构建海岛地区小康社会评价指标体系。在分析25个评价指标的计算方法和目标值的基础上,采用德尔菲法、分层构权法和循环法确定评价指标权重,据此对样本海岛地区小康社会子目标和总实现程度进行评价。结果表明,样本海岛地区小康社会总体实现程度均超过70%,处于良好水平。