An In Vitro Study of the Interaction of Copper(II) Salicylates with Genomic DNA Using Gel Electrophoresis and Gel Permeation Chromatography

This papers describes the in vitro interaction of copper(II) acetylsalicylate and copper(II) salicylate with genomic DNA isolated from human blood. The two drug substances were found to bind to DNA after incubation with whole blood over night. Bonding was confirmed by detection of separated DNA electrophoresis bands for copper, copper(II) acetylsalicylate, copper(II) salicylate, acetylsalicylic acid and salicylic acid. Drug–DNA interactions were observed during electrophoresis in the form of fragmentation by formation of two bands when compared to controls. Gel permeation chromatography parameters also confirmed the occurrence of fragmentation. The use of gel permeation chromatography parameters as a measure of fragmentation of DNA is discussed. The fragmentation of genomic DNA after incubation with copper(II) acetylsalicylate and copper(II) salicylate suggested that these drug substances might be responsible for cytotoxicity in vivo.

     

Characterization of Polyphenylene Sulfide Using Gel Permeation Chromatography with Triple Detection

The increasing world demand for polyphenylene sulfide (PPS) due to its unique properties has augmented the pressure on development of analytical methods to evaluate its molecular weight distribution and structure. Whilst gel permeation with triple detection (GPC3D) has been considered for PPS analysis, its development and effectiveness has been impaired because of, firstly, the high temperature needed to maintain solubility (>205°C), and, secondly, a very low dn/dc for the polystyrene calibration standards in 1-chloronaphthalene. This article presents practical recommendations to overcome these early difficulties by discussing the results obtained on PPS samples analyzed with a commercially available GPC3D instrument.     

Characterization of Bituminous Compounds by Gel Permeation Chromatography (GPC)

Abstract

Gel permeation chromatography is applied to the qualitative and quantitative characterization of asphalt, asphaltenes and maltenes. The nature of their molecular size distributions, micellar dimensions, and degree of aromatic polycondensation are described. The resultant data are used to provide insight into the nature of associative processes involving these materials.     

同步荧光光谱法研究明胶蛋白质与铜(II)的相互作用

利用同步荧光光谱技术,研究了pH为10.0时,Cu2+离子与明胶的相互作用,推导出含有n个键合位置的明胶大分子与Cu2+离子的结合公式;用明胶中两种荧光基团的荧光强度变化数据,线性拟合出Cu2+离子与明胶的结合常数K和结合位点数n.讨论了Cu2+离子对明胶分子构象的影响.非线性拟合结果与实验值相当吻合.     

Analysis of the Molecular Weight Distributions of Aminolyzed Poly(Ethylene Terephthalate) by Using Gel Permeation Chromatography

The molecular weight distributions of poly(ethylene terephthalate) fibers aminolyzed with selected primary amines (namely, methylamine, ethylamine, n-butylamine, and ethanolamine) were determined by using gel permeation chromatography. Initially the shape of the differential molecular weight distribution (DMWD) curve did not change although its peak shifted to lower molecular weights. As aminolysis continued, a shoulder appeared on the DMWD curve. Its appearance seemed to coincide with an increase in the density of the product. Ultimately, distinct molecular populations could be identified in the treated polymer depending on the severity of the aminolysis and the selectivity of the particular amine. The lowest is thought to represent primarily crystalline residues and has a peak molecular weight of 3400. The relations between M _n and ultimate tenacity and breaking strain for the aminolyzed products were linear.     

Voltammetry and Spectroscopy Study of In Vitro Interaction of Fenitrothion with DNA

The interaction of Fenitrothion with DNA has been studied using the voltammetric and spectroscopic methods. An irreversible reduction was concluded from the CV data of Fenitrothion. The values of (αn)_f=1.91 and (αn)_b=2.06 were measured and the reduction process of Fenitrothion was performed with 4 electrons. By using non‐linear regression analysis of CV data, the binding constant, binding site size, and diffusion coefficient for free Fenitrothion (D_f) and DNA‐Fenitrothion (D_b) were calculated as: 1.03×10⁴, 1.204, 5.2×10^?4 and 1.72×10^?5, respectively. Also the voltammetric, spectroscopic, thermodynamic and activation energy of DNA‐Fenitrothion complex revealed that the mode of interaction might be partial‐intercalative and complex formation is entropy favored.     

液体色谱,凝胶色谱分析低聚芳砜及其双烯大分子单体

本文用液相色谱和凝胶色谱对双酚A、双酚S型低聚芳砜及α,ω-双甲基丙烯酸聚芳砜酯大分子单体进行了组分分析,通过改合成条件、测定数均分子量等辅助手段确定液相色谱各峰的归属,计算其分子量及分子量分布指数,并对两种方法测定的结果进行了比较。用液相色谱观察低聚体每个组分的含量及其反应过程中的消长情况比凝胶色谱清晰。     

高效凝胶渗透色谱法研究超氧化物歧化酶的分子量

本文采用凝胶渗透色谱仪，对修饰后的牛血ＳＯＤ进行测定。仪器：美国ＷａｔｅｒｓＡＬＣ／ＧＰＣ２４４型高效液相色谱仪，ＳｈｏｄｅｘＰ－８２葡聚精为高分子标样。采用紫外和示差折光双检测器进行测定。所得数据与经典的凝胶电泳法完全一致，为此类高分子材料的Ｍｎ、ＭＷ和Ｄ值的测定，建立了准确、快速的测定方法。     

凝胶渗透色谱-气相色谱质谱法测定：花生中6种除草剂农药残留

建立了凝胶渗透色谱一气相色谱质谱（GPC～GC=MS）法测定花生中6种除草剂（氟乐灵、异恶草酮、甲草胺、二甲戊乐灵、乙氧氟草醚、喹禾灵）农药残留的方法。样品经乙腈提取,氨基固相萃取柱和凝胶渗透色谱净化,在选择离子扫描（SIM）模式下进行气相色谱质谱法测定,外标法定量。6种除草剂浓度在0．02-1．00mg／L范围内与色谱峰面积呈良好的线性,线性相关系数为O．9949～0．9998,添加回收率为77．8％-101．6％,测定结果的相对标准偏差为4．4％～11．4％（月=5）,方法的检出限为0．1～1．3μg／kg。     

四氮大环-金属配合物与DNA作用的电化学及谱学研究

Mononuclear copper（Ⅱ）, nickel（Ⅱ） and cobalt（Ⅲ） tetracoordinate macrocyclic complexes were synthesized and spectroscopically characterized. The crystal structure of the three compounds were determined by X-ray crystallography. The electrochemical experimental results indicate that the three complexes could interact with DNA mainly by electrostatic interaction. The interaction of tetracoordinate macrocyclic cobalt（Ⅲ） complex with DNA was studied by cyclic voltammetry and UV-vis spectroscopy. The experimental results reveal that tetracoordinate macrocyc- lic cobalt（Ⅲ） complex could interact with DNA by electrostatic interaction to form a 1 ： 1 DNA association complex with a binding constant of 7.50 ×10^3 L·mol^-1.     

Studies on the Electrochemical Property of Dinuclear Copper(II) Complex Containing Dimethylglyoxime and Its Interaction with DNA

The electrochemical property of dinuclear copper(II) complex containing dimethylglyoxime [Cu₂(Hdmg)₄] was studied with cyclic voltammetry. Cu₂(Hdmg)₄ had an irreversible oxidation peak in pH 5.0 B–R buffer solution at the stearic acid‐modified carbon paste electrode. Cyclic voltammetry, UV‐vis absorption spectra and viscosity measurements were used to study the interaction of Cu₂(Hdmg)₄ with herring fish sperm DNA. Cu₂(Hdmg)₄ interacts with the bases of DNA to form nonelectroactive adducts. The interaction of Cu₂(Hdmg)₄ with ssDNA was stronger than that of Cu₂(Hdmg)₄ with dsDNA because of the exposed bases of ssDNA. The gene sequence related to the BAR transgene in the transgenic corn was detected using Cu₂(Hdmg)₄ as electroactive indicator.     

An In Vitro Investigation of UHMWPE Modified with Cu (II) Chelate of Bissalicylaldehyde-Ethylenediamine

This article investigates the performance of ultra high molecular weight polyethylene (UHMWPE) modified with 15 wt% Cu (II) chelate of bissalicylaldehyde-ethylenediamine, a type of Schiff base copper complex that has antibacterium and antitumor activity, as a potential artificial hip joint material. The modified UHMWE demonstrated excellent tribological and biocompatible properties, and a higher wear resistance, a better thermal conductivity and increased deformation resistance as compared to pure UHMWPE.     

Optimization of Peak Separation and Broadening in Aqueous Gel Permeation Chromatography (GPC) -Poly (Sodium Styrene Sulfonates)

Abstract

An experimental study of the gel permeation chromatography of a series of poly (sodium styrene sulfonates) in aqueous media has been undertaken. The objective of this study was to develop a set of operating conditions that would maximize peak separation and minimize peak broadening. Using CPG-10 porous glass packing, it has been found optimal to work at pH near 6 and ionic strength near 0.05. Under those conditions, ion exclusion is eliminated and the optimum balance between resolution and reproducibility is obtained. Addition of a few ppm neutral surfactant to the mobile phase prevents adsorption to the packing surface, and improves resolution.     

双马来腈二亚胺合铂与DNA的作用

本文以紫外-可见光谱、荧光光谱及黏度法研究了双马来腈二亚胺合铂与DNA的作用。紫外-可见光谱的研究表明,与DNA作用后,双马来腈二亚胺合铂在可见区的吸收显示出了减色效应,并伴随着吸收峰的蓝移。Scatchard图的分析结果表明,双马来腈二亚胺合铂与DNA的作用位点与溴化乙锭不同。黏度法实验表明,双马来腈二亚胺合铂与DNA作用后降低了DNA的相对黏度。这些研究结果表明,双马来腈二亚胺合铂以静电作用方式与DNA结合。本研究有助于深入理解双马来腈二亚胺合铂的作用机理并开发这种潜在的新型光动力治疗剂。     

Polyvinylacetate Gel Permeation Chromatography of H-Coal Liquids and Model Compounds. Comparison with Rigid Gel,Reversed Phase and Normal Phase Chromatography

Abstract

This paper reports the application of polyvinylacetate gel (Fractogel) for size fractionation of the H-Coal liquids and model aromatic hydrocarbons. The four H-Coal liquids were each divided into three classes according to solubility in hexane, benzene, and pyridine. A model mixture of eight compounds when applied to the Fractogel column yielded four fractions; a similar performance was given by a prepacked, Toyo Soda microparticulate column containing styrene-divinylbenzene copolymer. Regarding the twelve H-Coal solvent fractions, the chromatograms obtained from the Fractogel column were analogous to those from the Toyo Soda column. By making further use of model compounds, the Fractogel results are compared with those obtained from reversed phase chromatography on a Partisil ODS column and those from normal phase chromatography on a LiChrosorb silica column. These comparisons reveal the usefulness in separating certain aromatic hydrocarbons by the Fractogel column. Furthermore, judging from the chromatograms of a hexane-soluble H-Coal fraction obtained by the reversed phase and normal phase methods, the ODS column will complement the Fractogel column in fractionating the H-Coal liquids.     

加速溶剂提取凝胶渗透色谱净化气相色谱质谱快速测定玉米中多环芳烃

研究了玉米中16种多环芳烃的快速分析方法.采用加速溶剂萃取法(ASE)对玉米样品进行提取,提取溶剂为二氯甲烷,萃取池中依次加入3 g中性氧化铝吸附剂和10 g待测样品,提取的同时能够在线净化除去小分子杂质.收集的提取液进一步用凝胶渗透色谱(GPC)除去样品中大分子油脂和色素,流动相为二氯甲烷,流速为3 mL/min,收集9～13 min的流出液,提取液浓缩定容至1 mL后用GC-SIM-MS进行分析.16种 PAHs以及4种替代物在2个浓度水平添加时的平均添加回收率在55.7%～145.3%之间; RSD为1 4%～16.8%;方法检出限为0.005～0.120 ng/g.本方法简便、快速、准确,净化效果较好,满足残留分析的要求,且能应用于其它谷物样品的日常分析.     

Interaction of Double-Helical Polynuclear Copper(I) complexes with double-stranded DNA

Double-helical metal complexes, the helicates H₂–H₅ , were found to bind to double-helical DNA by spectroscopic, DNA-melting, and electrophoretic-mobility measurements. The helicates also inhibited the cleavage of DNA by two restriction enzymes, Sspl and EcoRV, a property which agrees with the binding occurring in the major groove of the double helix. Visible-light irradiation of solutions containing a helicate and the pBR322 plasmid led to single-strand cleavage, indicating that these complexes could be of interest as potential probes for nucleic-acid structure.     

铜离子与SALI3-2蛋白的相互作用

用1/2 MS固体培养基培养拟南芥幼苗, 研究了CuCl₂对转Sali3-2基因植株生长的影响, 发现转基因植株Sali3-2的表达可提高其耐受Cu²⁺胁迫的能力. 进一步克隆Sali3-2基因, 表达并纯化了缺失信号肽的 SALI3-2 蛋白. 利用固定金属离子亲和色谱(IMAC)分析发现, Cu²⁺ 能够与 SALI3-2 蛋白结合. 通过荧光光谱及圆二色光谱(CD)进一步研究了Cu²⁺ 与 SALI3-2 蛋白间的键合机理. 结果表明, Cu²⁺ 可引起SALI3-2 蛋白内源性荧光猝灭, 其猝灭机制为静态猝灭; Cu²⁺ 与SALI3-2 蛋白的结合常数为8.89×10⁶, 结合位点数为1.6. CD分析显示, Cu²⁺ 与SALI3-2 蛋白的结合未使SALI3-2 蛋白二级结构发生明显改变. 由此推测, 在高浓度铜离子胁迫下, SALI3-2蛋白通过结合一定数量的Cu²⁺使蛋白的构象发生改变, 这可能是SALI3-2蛋白的表达使植物耐受Cu²⁺胁迫能力提高的分子机制之一.     

Interaction of Palladium(II) Acido Complexes with DNA

Interaction of K₂[PdCl₄] (I) and (C₅H₁₂NO)₂[PdCl₄] (II) with DNA in vitro is studied. No fragmentation of DNA occurs under the action of II. The interstrand cross-links are formed due to the formation of complexes with purine and pyrimidine bases; no interaction with DNA phosphates is observed. The cation does not play an essential role in the formation of cross-links.     

Study of the Interaction of Bis(4‐pyridylthio)methane with Copper(II) Chloride and Bromide

The new ligand bis(4‐pyridylthio)methane (4‐bpytm) ( 1 ) and its complexes [CuX₂(4‐bpytm)] and [CuX₂(4‐bpytm)₂] (X = Cl and Br) ( 2 – 5 ) have been prepared and characterized by elemental analysis, IR‐Raman, UV/Vis spectroscopy. The structures of (4‐bpytm) ( 1 ), [CuCl₂(4‐bpytm)₂] ( 3 ) and [CuBr₂(4‐bpytm)₂] ( 4 ) were determined by single‐crystal X‐ray diffraction analysis. X‐ray analysis of the 1:2 derivatives reveals that the copper atom has a distorted (4 + 2) octahedral environment. The copper atom is coordinated by four nitrogen atoms from four bridging 4‐bpytm ligands and two halogen atoms. The axial Cu–N bonds are considerably longer than the equatorial Cu–N bonds owing to JahñTeller distortion. CuX₂ units are linked to each other through bridging 4‐bpytm ligands to form a 2D interpenetrated coordination polymer. The structural parameters of the 4‐bpytm ligand in these complexes were compared with those of the free ligand.