光度显色剂8-羟基喹啉-5-磺酸的纯化方法

报道了8-羟基喹啉-5-磺酸硅胶干柱层析纯化方法，探讨了固定相、淋洗剂、洗脱剂对产品纯化的影响，确定了以层析硅胶为固定相，以V(正(异)丙醇)：V(氨水)＝2：1为淋洗剂，以蒸馏水为洗脱剂的纯化条件。经过红外光谱和高效液相色谱分析证明，使用本方法可获得纯度大于99％的产品，结果满意。     

7-碘-8-羟基喹啉-5-磺酸与钒显色反应的研究及应用

在 0 .2 0mol·L- 1硫酸介质中 ,用过氧化氢作增敏剂 ,7 碘 8 羟基喹啉 5 磺酸 (Ferron)与钒 (Ⅴ )形成 1∶1的有色配合物 ,在 4 10nm处有最大吸收 ,其表观稳定常数为 4 .5× 10 3 ,摩尔吸光系数ε4 10 为 1.91× 10 3 L·mol- 1·cm- 1,钒浓度在 0 .10～ 2 0 .0 μg·ml- 1范围内符合比耳定律。该方法用于矿样中钒的测定 ,结果满意     

镉（Ⅱ）—7—碘—8—羟基喹啉—5—磺酸络合物吸附波的研究

在ｐＨ４．３的ＨＡｃ－ＮａＡｃ介质中，Ｃｄ（Ⅱ）与７－碘－８－羟基喹啉－５－磺酸（７－Ｉ－Ｈ２ＱＳ）生成络合物。有二苯胍存在下，于－０．６８Ｖ（ｖｓ．ＳＣＥ）产生一灵敏的极谱波，峰电流与Ｃｄ（Ⅱ）浓度在８．９×１０－９～２．２×１０－６ｍｏｌ／Ｌ浓度范围内呈线性关系。通过对该极谱波性质及反应机理的研究，证实其为络合物吸附波，络合比为１∶１，络合物带负电荷。方法用于铜矿中镉的测定，结果满意     

铋(Ⅲ)-8-羟基喹哪啶体系极谱行为——表面活性剂增敏机理和分析应用——Ⅱ.铋(Ⅲ)-8-羟基喹哪啶络合物电极反应和十二烷基苯磺酸钠增敏机理

试验表明,铋(Ⅲ)-8-羟基喹哪啶(8-OXQ)络合物(pHll,-0.60V)的峰电流(p)具吸附特性,为准可逆电极反应过程,其电子转移数(n),传递系数(α)及饱和吸附量(Γ_ο)分别为3,0.45,6.5×10~(-12) mol/cm~2。加入十二烷基苯磺酸钠(SDBS)未形成三元络合物,因SDBS的超载强烈吸附,引起诱导吸附,电双层结构激烈变化,而使电流峰形巨变,电流峰高(i_p)增大10余倍。讨论并指出SDBS对Bi(Ⅲ)与8-羟基喹啉(8-OX)及衍生物络合吸附电流增敏或抑制,与试剂组分、结构、解离态及络合物存在状态、电荷数、符号有关。     

钴-8-羟基喹啉-5-磺酸的荧光光度法的研究及应用

以8-羟基喹啉-5-磺酸测定金属离子的荧光反应已有报道。我们研究了CoH₂O₂-8-羟基喹啉-5-磺酸(H₂QS)体系,钴含量在3.7×10^-7～2.5×10^-5mol/L时,该方法能给出线性响应,试验了多种离子的干扰情况,拟定了植物样品中微量钴的测定方法,初步探讨了反应机理。     

取代8-羟基喹啉钌络合物催化Friedl?nder反应合成喹啉衍生物

Friedl?nder喹啉合成法是以邻胺基芳基醛或酮与有α-亚甲基的酮环化制备喹啉的反应,报道了一种喹啉钌络合物催化Friedl?nder法合成喹啉的方法.首先,以8-羟基喹啉钌络合物为催化剂,对模板反应邻氨基苯甲醇和苯乙酮合成2-苯基喹啉进行了反应条件优化实验.重点对比研究了8-羟基喹啉钌络合物配体上不同取代基对反应收率的影响,其中5-甲基-8-羟基喹啉(1e)钌络合物催化邻氨基苯甲醇和苯乙酮合成2-苯基喹啉获得了73%的最高收率.结合IR, UV以及密度泛函理论(DFT)计算讨论了配体结构与催化性能之间的关系.提出了β-H消除形成醛过渡态,交叉aldol反应再亚胺环化,最后脱水生成目标产物的可行机理.以(1e)₃Ru为催化剂,在优化的反应条件下进行了底物扩展研究,以69%～94%的收率合成了32个不同取代的喹啉衍生物,验证了方法的普适性.     

铜-高铁试剂络合物吸附催化波及十二烷基苯磺酸钠增敏机理

研究了在没有及含有十二烷基苯磺酸钠(SDBS)存在的0．1mo1/L NaHCO3底液中，铜(Ⅱ)-高铁试剂络合物的电化学行为。由于与十二烷基苯磺酸钠共吸附在电极表面上的超氧阴离子自由基氧化了电极反应中间体，产生了催化电流。     

8-羟基喹啉-5-磺酸金属络合物的荧光特性及其应用研究

本文报道了8-羟基喹啉-5-磺酸的金属络合物在不同条件下的荧光特性,探讨了使用激光-时间分辨技术,建立镁、铝荧光分析方法的可能性.     

极谱络合催化波测定钯

在Na2 CO3 NaHCO3 (pH 8.6 )缓冲溶液中 ,钯 与 8 羟基喹啉 5 磺酸形成的络合物在有阴离子表面活性剂十二烷基硫酸钠存在时 ,于 - 0 .72V(vs.SCE)处有一个二阶导数极谱波 ,与没有十二烷基硫酸钠存在时相比 ,峰电流增敏约 30倍 ,钯 浓度在 7.5× 10 -9～ 2 .8× 10 -6mol/L范围内 ,i″p 与钯 的浓度呈线性关系 ,检出限为 2 .8× 10 -9mol/L ,方法用于催化剂和工业废水中钯的测定 ,结果满意     

The Electrooxidation of Tetracycline at Acetylene Black Electrode in the Presence of Sodium Dodecyl Sulfate

The electrooxidation of tetracycline (TC) at acetylene black electrode has been studied in the presence of sodium dodecyl sulfate (SDS). Tetracycline (TC) exhibited very sensitive oxidation peak in this system. The peak current was proportional to TC concentration, and the detection limit was 1.2×10-8 mol/L. The system was used to the determination of TC in Pharmaceuticals.     

8-羟基喹啉-5-磺酸修饰电极pH传感器的制备及应用

制备了8-羟基喹啉-5-磺酸(HQS)修饰铂丝电极pH传感器,对其pH响应范围,斜率,线性相关系数,响应时间等进行了考察.将该电极用于表面修饰氨基纳米二氧化硅的测定,取得了满意结果.     

Sensitivity Improvement of the Oxidation of Tetracycline at Acetylene Black Electrode in the Presence of Sodium Dodecyl Sulfate

The oxidation of tetracycline (TC) was investigated at an acetylene black electrode in the presence of sodium dodecyl sulfate (SDS). TC exhibited a sensitive oxidation peak in the medium system, which was attributed to the enhanced adsorption of protonated TC at the negatively charged SDS film on the electrode surface. The mechanism of the electrode process was discussed, and some experimental conditions were optimized. The oxidation peak current was proportional to TC concentration in the range of 1.2×10^?7–6.0×10^?5 M, and based on three times the background signal, a detection limit of 1.2×10^?8 M was obtained for 150 s accumulations. The method has been used to determine TC in honey and pharmaceutical, and the results compared favorably.     

亚甲蓝与十二烷基硫酸钠变色反应光谱机理

为从分子水平认识亚甲蓝(MB)分子与大分子之间相互作用机理,应用吸收光谱法研究了MB与十二烷基硫酸钠(SDS)之间相互作用机理,考察了乙醇、氯化钠、羟丙基-β-环糊精以及Triton X-100对相互作用的影响。结果表明:MB与SDS之间能发生相互作用形成复合物产生变色反应,乙醇等对相互作用都有影响。认为MB与SDS变色反应机理是在MB与SDS大分子间发生静电相互作用基础上,结合在SDS有序集合体上MB分子定向聚集所引起的。     

十二烷基磺酸钠对大豆过氧化物酶活性和构象的影响

在不同的pH值体系中, 利用酶活测量、圆二色谱、荧光谱和电子吸收谱研究了十二烷基磺酸钠(SDS)对大豆过氧化物酶(SBP)活性与构象的影响情况. 在pH 2.6和4.2 的体系中, 少量的SDS分子可通过静电作用与SBP结合, 进而与SBP分子中的His169残基结合, 降低其与铁卟啉的配位能力, 使其Soret吸收带蓝移, 二级结构发生轻微的变动, 活性永久丧失. 在pH 5.2体系中, SDS和SBP分子都带负电, 由于静电排斥作用, SDS无法进入SBP的分子内部, 失去与SBP分子中His169残基结合的能力, 对SBP分子的二级结构没有影响, 仅对SBP分子的三级结构有所影响. 当SDS的浓度大于临界胶束浓度时, 由于胶束与SBP的静电排斥作用增强, 限制了铁卟啉中乙烯基的运动, 乙烯基与卟啉环的共轭程度增大, Soret 吸收带红移. 由于SBP活性可完全恢复, 此变化是可逆的.     

Growth Mechanism of Large Monodispersed Silica Particles Prepared from Tetraethoxysilane in the Presence of Sodium Dodecyl Sulfate

Monodispersed silica particles up to ca. 1.2 μm in diameter were prepared by hydrolysis of tetraethoxysilane in the presence of sodium dodecyl sulfate (SDS). The particle size was increased with an increase of SDS added. The geometrical standard deviation of the particles was decreased with an increase of SDS. In the earlier reaction stage, double spherical particles by the coalescence of the particles were frequently observed when large amounts of SDS were added. Particle size was gradually increased after the coalescence occurred and spherical particles were finally obtained. The results of Nielsen’s chronomal analysis suggest that the polynuclear layer growth took place after the coalescence of the particles in the presence of larger amount of SDS.     

Determination of Tyrosine in the Presence of Sodium Dodecyl Sulfate Using a Gold Nanoparticle Modified Carbon Paste Electrode

A carbon paste electrode modified with gold nanoparticles (AuMCPE) was used as a highly sensitive sensor for determination of Tyrosine (Tyr), in the presence of an anionic surfactant, sodium dodecyl sulfate (SDS), in aqueous solution. The measurements were carried out by using of differential pulse voltammetry (DPV), cyclic voltammetry (CV), amd chronocoulometry and chronoamperometry methods. The prepared electrode shows voltammetric responses with high sensitivity and selectivity for Tyr in the presence of SDS. The relationship between the oxidation peak current of Tyr and its concentration was obtained linearly and it was 1.0 × 10^?7 to 1.0 × 10^?5 M with a detection limit of 5.5 × 10^?8 M in the absence of SDS. On the other hand the oxidation peak current of Tyr increased significantly at AuMCPE in the presence of SDS and its detection limit was reduced to 2.7 × 10^?9 M. The proposed voltammetric approach was also applied to the determination of Tyr concentration in human serum.