聚丙烯酰胺超高相对分子质量测量不确定度评定

根据SY/T 5862–2008聚丙烯酰胺相对分子质量测量方法,测量了超高分子量聚丙烯酰胺的相对分子质量。经过对聚丙烯酰胺相对分子质量测量过程引入的不确定度进行分析和评定,不确定度的来源主要是试样目标液配制过程中引入的不确定度,其次是相对分子质量测量重复性、试样固含量的测定以及温度所引入的不确定度。聚丙烯酰胺相对分子质量测定结果为(2500.6±32.6)×104,k=2。     

温敏两亲性接枝物PAM-g-PNIPAm的合成及表征

以巯基乙胺为分子量调节剂,以丙烯酰氯作为链端转化剂合成了不同分子量的端丙烯酰胺基聚(N-异丙基丙烯酰胺)(PNIPAm)大分子单体;与丙烯酰胺共聚合,合成了以PNIPAm为侧链的接枝聚丙烯酰胺.用FTIR和¹HNMR方法表征了接枝聚合物与大分子单体的组成.该接枝聚合物在水溶液中具有热缔合特性及明显的温敏增稠性,水溶液的粘度在32～50℃之间随温度增加而增加.     

LaFe_(13-x)Si_x合金中不同铁磁态磁化率与磁场诱导磁相变的临界磁场实验研究

通过对采用不同方法制备或热处理的LaFe_(13-x)Si_x合金中处于不同磁状态的1∶13相磁化过程的观察和分析,实验研究了该系合金中各种铁磁态的最大磁化率,以及磁场诱导顺磁态到铁磁态的巡游电子变磁相变临界磁场与温度的关系。结果表明,在居里温度以下合金中铁磁态的最大磁化率,高于居里温度以上因磁场诱导由顺磁态相变而来的铁磁态的最大磁化率。居里温度附近两相共存态中的顺磁态,由磁场诱导转变为铁磁态的临界磁场,小于居里温度以上合金处于完全顺磁态时由磁场诱导转变为铁磁态的临界磁场随温度变化的线性关系外推值。且在两相共存态中,因磁场诱导的铁磁态的最大磁化率也小于合金中本身存在的铁磁态的最大磁化率。另外,当合金中1∶13相处于顺磁态和铁磁态两相共存时,经励磁-退磁至零场后转变为铁磁态,两相共存现象消失。     

顶空-气相色谱-质谱联用分析桂花和叶中挥发性成分

采用谱库检索结合准确质量测定、保留指数、串联质谱技术的多维定性分析策略鉴定化合物, 能够提高定性分析的效率和准确性. 运用顶空-气相色谱-四极质谱、顶空-气相色谱-飞行时间质谱以及顶空-气相色谱-串联质谱联用技术对桂花样品进行了分析检测, 并采用多维定性分析思路对检出的挥发性成分进行了鉴定. 结果共确认出47种挥发性成分, 其中单萜类和倍半萜类化合物为主要组分. 该定性分析策略准确可靠, 可以广泛应用于复杂样品挥发性成分的定性分析中.     

热响应纳米金球作为非共价药物载体合成及性质研究

以聚N-异丙基丙烯酰胺接枝的聚酰胺作为稳定剂,以纯水作为溶剂,采用原位合成的方法合成了具有可调光热响应行为、智能响应释药行为的有机无机杂化金纳米粒,并以TEM、紫外-可见分光光度计测定其在不同温度下分别对金核的粒径和表面等离子吸收峰的影响,采用1H-NMR,IR对上述聚合物做了表征.通过紫外-可见光分光光度计测定了不同组样品的低临界溶胀/溶解温度(LCST)值,发现不同组样品LCST有一定差别,通过激光照射测定了样品的体外光热响应性能.选用难溶性吲哚美辛作为模型药物,考察了各组样品的载药释药行为.实验研究结果表明,聚N-异丙基丙烯酰胺接枝的聚酰胺修饰的金纳米粒较单独的聚合物N-聚异丙基丙烯酰胺更适宜作为多功能药物载体:具有更接近人体生理温度的LCST值,并且具有随温度变化而发生变化的光热响应性质及温度响应的药物释放行为.因此它在难溶性药物的控制释药、光热肿瘤消融领域具有较为广阔的应用前景.     

丙烯酰胺共聚合及产物分散性的研究

采用水溶性引发体系研究了丙烯酰胺的均聚以及与几种乙烯基单体的共聚反应。探讨了引发剂、温度、单体浓度及加热时间对所得聚合物相对分子质量及其分散性能的影响。对产物的结构特性和相对分子质量分布进行了表征,并考察了共聚物的分散性能。丙烯酰胺共聚物同均聚物相比,分散性能有明显的改善。     

分散聚合法制备非离子型聚丙烯酰胺“水包水”乳液

利用丙烯酰胺在硫酸铵水溶液分散介质中的分散聚合制备了聚丙烯酰胺水溶性聚合物分散体;研究了硫酸铵浓度、聚甲基丙烯酰氧乙基三甲基氯化铵(PDMC)的相对分子质量及甲酸钠用量对聚丙烯酰胺水分散体系分散稳定性的影响.结果表明,获得稳定聚丙烯酰胺分散体系的最佳合成条件为:不加甲酸钠、PDMC的相对分子质量为8.02×105、硫酸铵的质量分数为20.9%.在最佳条件下得到的聚丙烯酰胺聚合物的相对分子质量为1.12×106.     

合成聚丙酰胺-硫属半导体复合纳米材料的新技术

在水溶液体系中采用同步聚合-水解技术（Simultaneous Polymerization-Hydrolysis）制备聚丙烯酰胺-半导体纳米复合材料。该SPH技术是基于丙烯酰胺单体的聚合和MS(M=Cd,Pb,Zn)纳米粒子的形成同步发生,使生成的半导体纳米粒子可均匀分散在聚丙烯酰胺基质中。该技术还为制备其它有机聚合物-金属硫化物纳米复合物提供了一种新途径。     

碳链接枝共聚物——Ⅲ.聚丙烯酰胺的均相氧化及其与苯乙烯接枝共聚反应

不久前我们曾报导了聚丙烯酰胺的水溶液在室温或55℃时有可能与过氧化氢发生均相氧化反应,形成聚丙烯酰胺大分子过氧化物.这种水溶性的聚丙烯酰胺大分子过氧化物可引发烯类单体的接枝共聚,得到相应的碳链接枝共聚物。利用这种简便的接枝方法不仅可以合成一系列具有综合性能的接枝共聚物新品种,而且对大分子过氧化物引发烯类单体接枝共聚反应历程的研究也具有一定意义。     

NIPAM共聚物多孔水凝胶的光引发RAFT合成及其溶胀性能

采用光引发可逆加成-断裂链转移(RAFT)方法,在室温下先合成了链端含有三硫代碳酸酯基的大分子链转移剂聚(N,N'-二甲基丙烯酰胺)(PDMAM),然后与N-异丙基丙烯酰胺(NIPAM)、N,N'-二甲基双丙烯酰胺(BIS)交联共聚合,并通过聚乙二醇的制孔作用制得PNIPAM-g-PDMAM梳型/多孔水凝胶.采用FTI...     

琼脂糖凝胶CL-6B亲和色谱法一步纯化蚯蚓半乳凝素

环节动物的S型凝集素在结构和生化性质上都有别于一般的S型凝集素,其在抗癌等研究方面的潜在价值重大。根据环节动物S型凝集素的性质,采用惰性分子筛填料Sepharose CL-6B（琼脂糖凝胶CL-6B）作为亲和色谱介质对蚯蚓S型凝集素进行了纯化。以2 mmol/L乙二胺四乙酸（EDTA）-MEPBS (4 mmol/L β-巯基乙醇,150 mmol/L NaCl,20 mmol/L 磷酸盐,pH 7.2)溶液作为平衡液,以氨水(150 mmol/L,pH 10.5)作为洗脱液得到的蛋白质经SDS-PAGE（十二烷基硫酸钠-聚丙烯酰胺凝胶电泳）、凝血实验及荧光检测等证明了其即为蚯蚓S型凝集素。该方法只需一个步骤即可从蚯蚓提取液中分离到纯的S型凝集素,比传统方法更加快捷高效,优越性明显。该方法的应用将有利于对环节动物S型凝集素的深入研究。     

Size-based separations of proteins by capillary electrophoresis using linear polyacrylamide as a sieving medium: model studies and analysis of cider proteins

Electrophoretic conditions to separate sodium dodecyl sulfate (SDS)-protein complexes according to their relative molecular mass by capillary electrophoresis (CE) using linear polyacrylamide as a sieving matrix were examined. Five purified proteins with relative molecular masses between 14 400 and 66 200 Da were separated on a coated fused-silica capillary with an internal diameter of 100 microm and an effective length of 24 cm (total length, 32.5 cm). Benzoic acid was added to the solution of purified proteins as internal standard; beta-mercaptoethanol was also added as reducing agent. The running buffer composition was 0.05 M tris(hydroxymethyl)aminomethane (Tris), 0.035 M aspartic acid, 0.1% m/v SDS, 4% m/v acrylamide, the resulting pH being 8.0. The applied voltage was 7 kV (reversed voltage polarity) in order to avoid high current intensities. Under optimized conditions, the five proteins were separated in less than 15 min, with a % relative standard deviation (RSD) between 0.2 and 0.4 for migration times in the same day. Good efficiency (values between 150 000 and 40 000 N/m) and resolution (values between 2 and 2.8) were obtained. The inverse of relative migration times was found to correlate with the logarithm of their relative molecular mass. Finally, cider proteins were analyzed and their relative molecular masses were determined. These results were compared with those obtained by SDS-polyacrylamide gel electrophoresis (SDS-PAGE).     

聚丙烯酰胺修饰Fe_3O_4磁性纳米粒子的制备与表征

首先通过化学处理在Fe3O4磁性纳米粒子表面引入Si—H键,然后通过选择性的硅氢加成反应制备了一个端基带溴的磁性引发剂,并利用原子转移自由基聚合(ATRP)技术,在该磁性引发剂表面接枝了聚丙烯酰胺高分子,该聚丙烯酰胺高分子展现出分子量高度可控性和窄的分子量分布.经聚丙烯酰胺修饰后Fe3O4磁性纳米粒子的比饱和磁化强度为58.5 emu.g-1,与未修饰纳米Fe3O4相比下降约20%.     

核壳型PVAc/PBA乳胶粒热力学平衡状态

乙酸乙烯酯;形态;核壳型PVAc/PBA乳胶粒热力学平衡状态;核壳结构;丙烯酸丁酯;乳液聚合;     

Design of a new,twelve-channel electrophoretic apparatus based on the Gradiflow technology

The Gradiflow technology, originally designed to carry out binary, size-based and charge sign-based electrophoretic protein separations, has been extended to simultaneously obtain multiple protein fractions from a single electrophoretic separation. The separation unit of the new apparatus houses the anode and cathode compartments and up to twelve shallow separation compartments through which the background electrolyte solution that contains the separated protein fractions is recirculated. The separation compartments are formed from grids as thin as 1.2 mm and polyacrylamide membranes as thin as 0.15 mm, all with corresponding multiple inlet and outlet ports. The average pore size of the polyacrylamide membranes can be varied to permit passage of proteins in the 5000-800 000 molecular mass range. The electric field, orthogonal to the flow paths of the recirculated background electrolyte, selectively moves the sample components across the polyacrylamide separation membranes. Selective protein transport can be achieved by exploiting differences in either the relative size of the proteins or the charge sign of the proteins. The advantages of the new apparatus stem from the synergistic combination of the short electrophoretic transfer distances, high electric field strength, large effective surface areas of the separation membranes, and the great flexibility with which apparati containing one to twelve separation compartments can be created.     

Sodium dodecyl sulfate-capillary gel electrophoresis of proteins using non-cross-linked polyacrylamide.

Proteins with relative molecular masses of 14,000 to 205,000 were separated by sodium dodecyl sulfate-capillary gel electrophoresis (SDS-CGE) using non-cross-linked linear polyacrylamide gels on both coated and uncoated fused-silica capillaries. It was determined that viscosity of the acrylamide solution was a major factor affecting column stability with linear acrylamide gels. When the viscosity of the acrylamide solution reaches 100 cP, electro-osmotically driven displacement of the gels is insignificant. Uncoated capillaries provided better resolution, stability, and reproducibility than surface coated capillaries when the concentration of linear polyacrylamide was greater than 4%. At lower gel concentrations, non-cross-linked polyacrylamide is easily displaced from the columns. A calibration plot of log molecular mass vs. mobility with non-linear polyacrylamide was linear, which indicated that resolution was equivalent to that obtained with cross-linked acrylamide. Separations with model proteins indicated that baseline resolution between protein species that vary 10% in molecular mass can be achieved.     

Ultrathin-layer sodium dodecyl sulfate gel electrophoresis of proteins: effects of gel composition and temperature on the separation of sodium dodecyl sulfate-protein complexes

This paper discusses the effects of gel composition and separation temperature on the migration properties of fluorescein-5-isothiocyanate-labeled protein molecular mass markers (ranging from 20 100 to 205 000 Da) in automated ultrathin-layer sodium dodecyl sulfate (SDS) gel electrophoresis. The separation mechanism with the agarose and composite agarose - linear polyacrylamide, agarose - hydroxyethyl cellulose, and agarose - polyethylene oxide matrices were all found to comply with the Ogston sieving model in the molecular mass range of the protein molecules investigated. Our temperature studies revealed that electrophoretic separation of SDS protein complexes is an activated process and, in pure agarose and in composite agarose hydroxyethyl cellulose and agarose - polyethylene oxide matrices that the separation requires increasing activation energy as a function of the molecular mass of the separated proteins. On the other hand, when linear polyacrylamide was used as composite additive, the activation energy demand of the separation decreased with increasing solute molecular mass. The sensitivity of the laser-induced fluorescent detection of the automated ultrathin-layer electrophoresis system was evaluated by injecting a series of dilutions of the markers and was found to be less than 2.5 ng/band for the fluorophore-labeled protein.     

Fast molecular mass and size characterization of polysaccharides using asymmetrical flow field-flow fractionation-multiangle light scattering

Asymmetrical flow field-flow fractionation (asymmetrical flow FFF), connected on-line to multi-angle light scattering detection (MALS) was shown here to be an efficient method for size characterization of pullulan standards and dextrans ranging from 20 000 up to 2 000 000 in molecular mass. The characterization of molecular mass and the molecular mass distribution of these polysaccharides is often complex and may require different methods. Using asymmetrical flow FFF-MALS, information was obtained not only about molecular mass and molecular mass distribution but also about hydrodynamic size as well as radius of gyration and conformation. The analysis time was very short, often below 5 min. It was shown that the pullulan standards have a narrow molecular mass distribution compared to the more polydisperse dextrans. Obtained molecular masses and distributions were in good agreement with data from the manufacturer. The dextrans, especially at high molecular mass, were found to have a more compact structure than the pullulans in both water and 0.1 M NaCl.