水溶性凝胶渗透色谱法测定碱木素分子量

应用水溶性凝胶渗透色谱法测定了碱木素的分子量,与脂溶性凝胶渗透色谱法的测定结果基本一致。色谱柱为Ｕｌｔｒａｈｙｄｒｏｇｅｌ凝胶色谱柱,流动相为氢氧化钠溶液（ｐＨ１２）。系统考察了不同流动相对碱木素在凝胶柱上吸附的影响,结果发现,增大流动相离子强度有利于减少碱木素的吸附,但流动相的酸度对于碱木素吸附具有更重要的影响,ｐＨ值高时,碱木素吸附减弱。实验同时表明,高分子量的碱木素更易在凝胶柱上发生吸附。     

测定木素磺酸盐和磺化碱木素相对分子质量分布的凝胶色谱法

用水溶性流动相在Ultrahydrogel柱上测定了木素磺酸盐和磺化碱木素的相对分子质量及其分布。流动相的离子强度和 pH值对样品和标样的保留时间和峰面积都有显著的影响。根据色谱峰的位置、峰面积和样品的分离程度 ,确定以 pH=7.0的0.1mol/LNaNO3 溶液为适宜的流动相。     

麦草碱木素及其热化学降解产物相对分子质量分布的测定

以pH=10的0．1mol/L NaNO3溶液为流动相，在Ultrahydrogel柱上测定麦草碱木素及其热化学降解产物的相对分子质量分布，测定碱木素降解产物所用洗脱液宜用pH10的0．1mol/LNaNO3水溶液，比较了由于样品结构特性和物理性质差异而造成的流动行为的差异，并确定两种样品各自的色谱条件。     

凝胶渗透色谱法测定木素磺酸盐相对分子质量分布

1　引　　言用凝胶渗透色谱 (ＧＰＣ)测定木素磺酸盐相对分子质量和相对分子质量分布 ,国外早在 6 0年代起就有文献报道 ,但国内在这方面文献报道较少。本文使用示差折光和紫外检测器 ,分别获得木素磺酸钠和木素磺酸钙的色谱图 ,用激光光散射检测器和标定线两种方法计算样品的平均相对分子质量及相对分子质量分布 ,并探讨了影响结果的因素。2　实验部分2 .1　仪器与试剂　Ｓｐｅｃｔｒａ公司凝胶渗透色谱仪 ,配Ｐ10 0泵 ,ＴＳＫ ＧＥＬ柱 ,接ＤａｗｎＷｙａｔｔ公司ＤＳＰ多角度激光检测器(ＭＡＬＬＳ)和ＲＩ 15 0检测器 ;Ｗａｔｅｒｓ公司…     

小鼠血浆中染料木素水溶性代谢产物和染料木素脂肪酸酯的分离及测定

本文建立了小鼠灌胃染料木素单体后血浆中水溶性染料木素代谢产物和染料木素脂肪酸酯的分离及测定方法。血浆样品经乙酸乙酯萃取后上Sephadex LH-20柱,分别用体积比1∶1的正己烷/氯仿和甲醇洗脱,染料木素脂肪酸酯用脂肪酶酶解后转化成染料木素,水溶性代谢产物用葡萄糖醛酸酶及硫酸酯酶水解成染料木素,然后采用液相色谱串联飞行时间质谱(Q-TOF LC/MS)检测染料木素。血浆中染料木素在10～10000 ng/mL范围内线性关系良好,检测限为1 ng/mL。10批次小鼠血浆中水溶性代谢产物平均为526.006 ng/mL,染料木素脂肪酸酯平均为58.976 ng/mL。采用SephadexLH-20柱具有良好的分离效果,脂肪酶水解染料木素脂肪酸酯稳定、专一性强,用Q-TOF LC/MS检测染料木素快速、灵敏。     

高效液相色谱法测定北五味子中5种木脂素含量

应用高效液相色谱法测定北五味子中五味子醇甲、五味子酯甲、五味子甲素、五味子乙素和五味子丙素等5种木脂素的含量。北五味子样品(1.000g)在70℃温度下用甲醇(20mL)微波辅助提取5min。分取部分提取液,以Hypersil ODS C18色谱柱为固定相,用乙腈和水以不同比例混合的溶液为流动相进行梯度洗脱,在检测波长225nm处进行测定。5种木脂素在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.029 2~0.050 7mg·L-1之间。以样品为基体,在3个浓度水平加入混合标准溶液进行回收试验,测得回收率在95.3%~101%之间,测定值的相对标准偏差(n=6)在1.1%~2.4%之间。     

凝胶色谱法测定木素磺酸盐电氧化降解产物的相对分子质量分布

 在Waters ALC/GPC244凝胶色谱仪上,使用Waters μ-Ultrahydrogel柱和示差折光检测器,以聚乙二醇作标样,测定了木素磺酸钙的电氧化降解产物的相对分子质量及相对分子质量分布。研究了流动相的电解质种类、离子强度和pH值对标样及试样色谱行为的影响。通过实验确定流动相为0.05 mol/L LiCl溶液,其pH值为6.5。所建立的方法用于木素降解产物相对分子质量分布的测定,具有简便、快速和稳定的特点。     

用GPC测定木素分子量及分子量分布的研究概况

<正> 木素结构的探索和工业应用的研究是当代木材化学科研工作的重要课题。这些工作都和木素分子量及分子量分布密切相关。然而,在一般测定高聚物分子量及分子量分布的方法中,超离心法是曾被认为应用于木素分子量及分子量分布测定最成功的方法,但其最好的结果也还不足于推算出木素分子量分布的具体数据。用凝胶渗透色谱法(简称GPC)测定木素分子量及分子量分布是六十年代发展起     

凝胶渗透色谱法对桉木过氧化氢化学法化学机械浆制浆过程木素分子量变化的

利用凝胶渗透色谱法和元素分析法测定了尾叶桉酶解木素在过氧地化学机械浆（ＡＰＭＰ制浆及漂白过程分子量的变化。研究结果表明：由于ＨＯＯ的特殊作用制浆及漂白之后,浆中剩余木素的平均分子量相对有所增加。     

薄层扫描法测定槐角及槐角丸中染料木苷和总染料木素的含量

槐角(Fructus Sophorae)为豆科植物的干燥成熟果实,冬天采收,有人工栽培和野生,全国大部分地区有生产.槐角丸是由槐角、黄芩、枳壳、防风、当归、地榆组成的常用中成药,具有清肠疏风、凉血止血的功效.槐角在处方中是君药,而染料木素、染料木苷为槐角的主要成分,具有极强的抗癌活性、抗繁殖性、抗氧化性、抗菌和消炎作用.关于槐角丸的有效成分测定方法主要有紫外分光光度法测总黄酮,薄层色谱法测定芦丁和黄芩苷,高效液相色谱测定黄芩苷和测定染料木素.本文在硅胶G薄层色谱板上,采用双波长薄层扫描法建立了测定槐角、槐角丸中的染料木苷和总染料木素的分析方法.染料木苷和染料木素的薄层展开剂分别为三氯甲烷-甲醇-冰醋酸(2574)和三氯甲烷-甲醇-冰醋酸(1510.1),染料木苷和染料木素分别在0.5～3.0 μg和0.9～5.0μg范围内呈良好线性.该方法快速、简便,为中药槐角和中成药槐角丸的质量控制提供科学依据.     

Abrasive Stripping Voltammetric Studies of Lignin and Lignin Model Compounds

Lignin is potentially a major renewable, nonfossil source of aromatic and cyclohexyl compounds. In this study, we have investigated the abrasive stripping voltammetry of lignin and four lignin model compounds in the room temperature ionic liquids (RTILs) [C₄mim][NTf₂], [N_6,2,2,2][NTf₂] and [C₄mim][OTf] (where [C₄mim]⁺=1‐butyl‐3‐methylimidazolium, [N_6,2,2,2]⁺=n‐hexyltriethylammonium, [NTf₂]^?=bis(trifluoromethanesulfonyl)imide and [OTf]^? =trifluoromethanesulfonate) on a gold macrodisk and in 0.1 M H₂SO₄ and 0.1 M NaOH on a boron‐doped diamond (BDD) macroelectrode, with the hope of using the voltammetry to fingerprint the functional groups within the lignin molecule. The use of RTILs on metal electrodes, or either acidic or basic media in combination with BDD electrodes allows solvent systems with wide electrochemical potential windows, useful for studying voltammetry which may be difficult to observe in systems where early breakdown of the solvent occurs.     

Lignin nanocomposites

Lignin is a biopolymer and one of the main constituents of woody plants where it plays the role of lining agent and is comparable in this respect to cement in steel reinforced concrete. Polymer nanocomposites containing biopolymers such as cellulose, lignin, starch, proteins, etc. are the object of recent numerous studies and are known also as bio-nanocomposites. This paper deals with lignin use in various polymer nanocomposites. It presents the preparation and uses of nanolignin as a filler and lignin uses as a matrix or a matrix component in polymer nanocomposites.     

木素的氧化性氨化反应(英文)

在一定压力和温度条件下,木素大分子和氨发生反应,生成一些氮修饰木素.为了解反应过程中木素分子结构的变化,用13 C和1H - 13 C 2D -NMRHMQC技术检测了反应前后的分子谱图,结果显示反应过程中木素分子的碎裂化现象十分明显,很可能在氧化性氨化反应过程中,木素大分子表面基团发生了氧化性修饰,如一些侧链 -CH3 被氧化形成 -CHO和 -COOH等,然后这些基团与氨结合等;此外,芳香环结构可能通过粘康酸单体断裂形成一些酰胺类产物,但木素分子内部的高度缩合性结构没有明显的变化     

Electrochemistry of Klason Lignin

The possibility of the use of Klason lignin extracted from sunflower husks as a cathode-active material for primary lithium battery has been demonstrated for the first time. The chemical composition, morphological and physical features were characterized by X-ray energy dispersive spectroscopy, impedance spectroscopy, scanning electron microscopy, and infrared spectroscopy. Electrochemical behavior of Klason lignin vs. Li/Li⁺ was studied by galvanostatic discharge and cyclic voltammetry. The reaction mechanism in electrochemical system was discussed. The maximum specific capacity of Klason lignin amounted to 380 mAh g^–1 at a current density of 25 mA g^–1.     

磺化碱木质素和磺化碱木质素聚氧乙烯醚的溶液行为研究

分别制备了不同磺酸基含量的磺化碱木质素(SAL)、不同交联度和分子量的磺化碱木质素聚氧乙烯醚(SAL-PEG),采用动态光散射(DLS)法分别研究磺酸基含量和PEG非离子长链对SAL和SAL-PEG溶液行为的影响规律.结果表明,不同磺酸基含量(1.28~2.09 mmol/g)的SAL在1.0 g/L的水溶液中存在聚集行为,磺酸基含量的增加使SAL的分子舒展程度增加,聚集程度越弱;Na Cl的加入使SAL的分子舒展程度减小,聚集体发生解聚.不同PEG含量的SAL-PEG在1.0 g/L的水溶液中主要以单分子状态存在,聚集行为较弱,分子的流体动力学半径与其分子量和交联度成正比;Na Cl的加入使SAL-PEG的PEG非离子长链却被严重压缩,分子流体动力学半径显著减小,减小程度与其分子量和交联度成正比,但SAL-PEG的聚集程度仍然较弱.     

丹参木质素及其单体含量的测定

本文建立了一种准确、快速的检测丹参中木质素及其单体含量的方法.采用Klason法和紫外分光光度法分别对丹参根和茎中酸不溶性木质素(Klason木质素)和酸溶性木质素含量进行了测定;运用硫代酸解法并结合气相色谱-质谱法(GC-MS)分别对丹参根和茎中各木质素单体组成进行了分析.结果显示,总木质素在丹参根和茎中的含量分别为...     

Effects of Alcell Lignin Methylolation and Lignin Adding Stage on Lignin-Based Phenolic Adhesives

To investigate the effects of lignin methylolation and lignin adding stage on the resulted lignin-based phenolic adhesives, Alcell lignin activated with NaOH (AL) or methylolation (ML) was integrated into the phenolic adhesives system by replacing phenol at various adhesive synthesis stages or directly co-polymerizing with phenolic adhesives. Lignin integration into phenolic adhesives greatly increased the viscosity of the resultant adhesives, regardless of lignin methylolation or adding stage. ML introduction at the second stage of adhesive synthesis led to much bigger viscosity than ML or AL introduction into phenolic adhesives at any other stages. Lignin methylolation and lignin adding stage did not affect the thermal stability of lignin based phenolic adhesives, even though lignin-based adhesives were less thermally stable than NPF. Typical three-stage degradation characteristics were also observed on all the lignin-based phenolic adhesives. Three-ply plywoods can be successfully laminated with lignin based adhesives, and it was interesting that after 3 h of cooking in boiling water, the plywoods specimens bonded with lignin-based phenolic adhesives displayed higher bonding strength than the corresponding dry strength obtained after direct conditioning at 20 °C and 65% RH. Compared with NPF, lignin introduction significantly reduced the bonding strength of lignin based phenolic adhesives when applied for plywood lamination. However, no significant variation of bonding strength was detected among the lignin based phenolic adhesives, regardless of lignin methylolation or adding stages.     

Effect of Lignin Structure Characteristics on the Performance of Lignin Based Phenol Formaldehyde Adhesives

As the second most abundant biopolymer, lignin remains underutilized in various industrial applications. Various forms of lignin generated from different methods affect its physical and chemical properties to a certain extent. To promote the broader commercial utilization of currently available industrial lignins, lignin sulfonate (SL), kraft lignin (KL), and organosolv lignin (OL) are utilized to partially replace phenol in the synthesis of phenol formaldehyde (PF) adhesives. The impact of lignin production process on the effectiveness of lignin-based phenolic (LPF) adhesives is examined based on the structural analysis of the selected industrial lignin. The results show that OL has more phenolic hydroxyl groups, lower molecular weight, and greater number of reactive sites than the other two types of lignins. The maximum replacement rate of phenol by OL reaches 70% w/w, resulting in organosolv lignin phenolic (OLPF) adhesives with a viscosity of 960 mPa·s, a minimal free formaldehyde content of 0.157%, and a shear strength of 1.84 MPa. It exhibits better performance compared with the other two types of lignin-based adhesives and meets the requirements of national standards.     

Untersuchungen über Lignin

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