黄嘌呤氧化酶－乙醛－吖啶酯化学发光分析新体系

乙醛在黄嘌呤氧化酶催化作用下，被空气氧化生成乙酸和过氧化氢，酶反应生成的过氧化氢氧化新吖啶酯试剂［１０－甲基－９－（对甲酰苯基）吖啶羧酸酯氟磺酸盐］产生化学发光，化学发光强度与己醛浓度在一定范围内成线性关系．由此建立了一种化学发光分析新体系，用于测定乙醇含量．线性范围２．０×１０－７～１．２×１０－３ｍｏｌ／Ｌ，测定５．０×１０－７ｍｏｌ／Ｌ乙醛，相对标准偏差为６．８％，检测限为１．２×１０－７ｍｏｌ／Ｌ，测定环境水样中乙醇含量，取得满意结果，回收率为９５～１０６％．     

5-甲氧基色醇-酸性高锰酸钾-甲醛化学发光体系研究与应用

在甲醛的存在下 ,5 -甲氧基色醇 (5 - ML)与高锰酸钾在高氯酸介质中发生化学反应 ,能产生很强的化学发光。本文据此采用流动注射技术研究其发光行为 ,对影响化学发光强度的实验因素进行优化 ,建立了快速灵敏测定 5 - ML的化学发光新方法 ,测定方法的线性范围为 2 .0× 10 -8mol/ L— 4 .0× 10 -5mol/ L,检出限为 7.9× 10 -9mol/ L(S/ N=3) ,相对标准偏差为 2 .4 % (5 .7× 10 -7mol/ L5 - ML;n=10 )。该方法应用于脑脊液样品中 5 - ML含量测定 ,回收率达到 86 .0 %— 97.2 %。文中还对体系的化学发光反应机理进行探讨     

化学发光法测定水中1-溴-3-氯-5,5-二甲基海因

基于在碱性条件下 (p H 12 .0— 12 .5 ) 1-溴 - 3-氯 - 5 ,5 -二甲基海因与鲁米诺 -过氧化氢体系反应产生化学发光的性质 ,建立了一种测定其含量的新方法。 1-溴 - 3-氯 - 5 ,5 -二甲基海因的浓度在 4 .0× 10 -8— 1.0×10 -6mol/ L范围内与化学发光强度呈良好的线性关系。本方法的线性范围宽 ,灵敏度高 ,检出限为 2 .0×10 -8mol/ L。操作简单、方便。应用于游泳池水中 1-溴 - 3-氯 - 5 ,5 -二甲基海因的测定 ,结果令人满     

测定抗坏血酸的流动注射化学发光新体系

基于在酸性介质中甲醛存在下 ,抗坏血酸与高锰酸钾直接化学发光反应 ,建立了测定抗坏血酸的流动注射化学发光的方法 ,该法测定抗坏血酸的线性范围为 3.0× 10 -8— 2 .0× 10 -5mol/ L,检出限为 1.0×10 -8mol/ L ,相对标准偏差为 2 .5 % (1.0× 10 -5mol/ L抗坏血酸 ,n=11)。该法应用于测定维生素 C针剂及片剂中抗坏血酸的测定 ,结果令人满意。     

光泽精化学发光体系的研究与应用

对光泽精化学发光体系的动力学性质、荧光光谱、化学发光光谱及化学发光机理进行研究和探讨。详细研究了光泽精 - H2 O2 - Co( )流动注射化学发光体系的最佳分析条件。结果表明 ,当光泽精 (L c)为 2 .5×10 - 5mol/L、H2 O2 为 0 .5 mol/L、Na OH为 0 .4 mol/L、CTMAB为 2 .0× 10 - 5mol/L时 ,测定 Co( )的校准曲线线性范围为 0 .0 5— 2 0 0μg/m L ,检出限为 0 .0 1μg/m L。对 10μg/m L Co( )连续测定 7次 ,相对标准偏差为 1.7%。     

流动注射化学发光法测定邻苯二酚

基于在甲醛存在下 ,邻苯二酚与高锰酸钾在酸性介质中发生化学发光反应 ,建立了测定邻苯二酚的流动注射化学发光分析法 ,该法测定邻苯二酚的线性范围为 3.0× 10 -8— 1.0× 10 -5mol/L,检出限为 1.0× 10 -8mol/L,相对标准偏差为 3.5 % (1.0× 10 -6mol/L邻苯二酚 ,n=11)。该法应用于测定自来水中加入的邻苯二酚 ,结果令人满意     

鲁米诺化学发光熄灭法测定稀土镧的研究

本文研究了稀土La（Ⅲ）对Luminol-H2O2-Cr(Ⅲ)化学发光体系的熄灭效应，在此基础上建立了稀土镧的流动注射化学发光分析法，方法的检出限为4×10^-8mol/L；对于2×10^-7mol/L稀土镧标准溶液测定的相对标准偏差为3.0%（n＝11）；线性范围为1.0×10^-7-1.0×10^-4mol/L；相关系数大于0.9984，该法用于合成样品分析，结果满意。     

流动注射化学发光增强法测定焦性没食子酸

在较低 p H值的 Na OH介质中 ,焦性没食子酸对 Luminol- K3 Fe(CN) 6化学发光体系有很强的增敏作用 ,据此建立了焦性没食子酸的测定方法——流动注射化学发光增强法。该法的化学发光增强值 (ΔI)与焦性没食子酸浓度 (在 3.0× 10 -9— 1.0× 10 -6mol/ L范围内 )呈良好的线性关系 ,检出限为 1.0× 10 -9mol/ L(n=11) ,对 5× 10 -8mol/ L焦性没食子酸测定的相对标准偏差为 2 .8%。用于没食子酸热解产物中的焦性没食子酸测定 ,结果令人满意     

Meso-5,10,15,20-四(4-甲氧基苯基)卟啉荧光熄灭法测定铅

基于铅对荧光试剂 Meso- 5 ,10 ,15 ,2 0 -四 (4 -甲氧基苯基 )卟啉 (TMOPP)的荧光熄灭 ,建立了测定微量铅的荧光分析方法。在 p H9.5的 Tris- HCl缓冲体系中 ,最大激发波长和发射波长分别为 4 2 4 nm和6 5 7nm,测定铅浓度的线性范围为 5 .5 0× 10 -7— 7.5 0× 10 -5mol/ L,检出限为 8.5 0× 10 -8mol/ L。用于环境水样中铅含量的分析 ,结果满意。     

Co(1,10-phen·)32+-KIO4-鲁米诺化学发光体系与应用

本文研究了Co(1,10-phen·)32+配合物对KIO4氧化鲁米诺所产生的强化学发光反应.以1,10-phen·为配位体时,Co(Ⅱ)的检出限为8×10-8g/L,工作曲线响应浓度范围在1×10-6~1×10-4g/L,测定1×10-4g/LCo(Ⅱ)离子的相对标准偏差为2.5%.配合物化学发光法检测啤酒、维生素B12针剂中微量Co(Ⅱ)可获得满意结果.     

顺序注射化学发光分析法测定空气中的甲醛

基于碱性条件下甲醛对没食子酸-过氧化氢发光反应的增敏作用,建立了顺序注射与化学发光检测联用测定空气中甲醛的新方法。在选定的实验条件下,甲醛浓度与发光强度在1.0×10^-7~2.0×10^-3 mol/L范围内呈线性关系,相关系数0.999 3,方法的检出限(3σ)为5.0×10^-8 mol/L。对1.0×10^-6 mol/L的甲醛进行11次连续测定的相对标准偏差为2.1%,每小时可实现连续测定140次以上。方法的回收率为92.0%~108.0%,对环境标准样品中甲醛的测定结果与推荐值一致。     

Determination of Catechin in Aqueous Solution by Chemiluminescence Method

A method to determine catechin in aqueous solution by measuring chemiluminescence intensities using a stopped flow system has been studied. The lucigenin-hydrogen peroxide chemiluminescence reaction was chosen for the determination of catechin. Fe(II) ion was added to the chemiluminescence system to increase the sensitivity. The chemiluminescence intensity from the lucigenin system was increased by the addition of catechin. Effects of flow rates of reagent and sample and concentrations of lucigenin, hydrogen peroxide, Fe(II) ion and KOH were investigated. The calibration curve for catechin was linear over the range from 1.0×10⁻⁶ to 1.0×10⁻³ M and the detection limit was 3.0×10⁻⁷ M under the optimal experimental conditions.     

2,9-二甲基-1,10-菲咯啉的化学发光研究

本文阐明了试剂2,9-二甲基-1,10-菲咯啉(称为新铜灵)在金属离子诸如Cu(Ⅱ)、Pb(Ⅱ)、Fe(Ⅲ)和Ni(Ⅱ)作为催化剂各自存在下,可与过氧化氢在碱性溶液中产生一种绿色的化学发光反应。此化学发光反应的机理已在本文中进行讨论,并认为是由于Cu(Ⅱ)与新铜灵生成之络合物在此过程中进行催化反应而致使过氧化氢生成超氧基离子,而此超氧基离子随即与新铜灵试剂作用产生化学发光。此化学发光反应的产物已用薄层色谱法进行分离,并且分别用紫外、红外和荧光分光光度法进行测定。 此外,这种新的化学发光反应已在我们实验室进行了分析应用试验。用此化学发光体系来做Cu(Ⅱ)的测定也在本文中说明。此法测铜的检测下限为8×10-9克/毫升;线性范围是1×10-8到4×10-7克/毫升。对于0.1ppm之铜的测定而言,除适量的Co(Ⅱ),Mn(Ⅱ)、Ni(Ⅱ)、Cd(Ⅱ)和Cr(Ⅲ)之外,其余外来离子均无干扰。这一分析方法能够满意地用于铝合金中铜的测定。     

New bis[N-(4-pyridyl)-P-Toluene Sulfonamide] Palladium Dichloride a Novel Fluorophore for Determination of Lysine Amino Acid

Here, we are describing the study of the chemiluminescence arising from the reaction of bis (2,4,6-trichlorophenyl) oxalate (TCPO) system with new bis [N-(4-pyridyl)-p-toluene sulfonamide] palladium dichloride (BSPC) as a novel luminescent. The optimum concentrations of all reagents such as sodium salicylate (SS) as catalyst, hydrogen peroxide as oxidizing reagent and the relationships between the chemiluminescence intensity and concentrations of TCPO, SS, hydrogen peroxide and BSPC are reported. After optimization the required reagents, the system were used for determination of amino acid lysine, as an effective and selective quencher in the solution functioning in a Stern–Volmer fashion. This resulted in the development of a facile and highly sensitive chemiluminescence detection scheme for the determination of lysine in biological samples. Ultimately, estimating quenching constant K _q of 4.29?×?10³ M^?1 was successfully carried out. Under the optimal conditions, the evaluated lower and upper detection limits of measurable concentration of lysine are 1.17?×?10^?7 and 3.18?×?10^?4 M, respectively.     

一种新的测定诺氟沙星的化学发光分析法

基于在碱性条件下,诺氟沙星(NFLX)对鲁米诺-过氧化氢(Luminol-H2O2)化学发光体系的化学发光信号有强烈的抑制作用,建立了一种简单、快速、可连续测定诺氟沙星的流动注射化学发光分析新方法.该方法线性范围为7.0×10-8-1.0×10-6mol/L,检出限(3σ)为1×10-8mol/L,对3.0×10-7m...     

测定司帕沙星的化学发光分析方法

基于在氢氧化钠介质中,司帕沙星对luminol-H2O2化学发光体系有明显的抑制作用,结合流动注射分析技术,建立了流动注射化学发光法测定司帕沙星药物的新方法.在优化的实验条件下,测定司帕沙星的线性范围是1.0×10-7-1.0×10-5mol·L-1,检出限为1.0×10-8mol·L-1,相对标准偏差（1.0×10-7mol·L-1的司帕沙星,n=11）为1.4％.     

BPR氧化减色法测定过氧化氢亨利常数

利用冷阱收集气-液平衡管出来的气相过氧化氢,以及氯化血红素(Hemin)催化下溴邻苯三酚红(bromopyrogallolred,BPR)被过氧化氢氧化减色的分光光度法检测,测定了温度依赖的过氧化氢亨利常数。在10~35℃的范围内,过氧化氢亨利常数KH(mol·L-1·atm-1)表达为lnKH=a/T-b,其中a=7269±22,b=13·26±0·08,T为温度(K)。过氧化氢溶解焓ΔH为60·43±0·18kJ·K-1·mol-1。     

Determination of Epinephrine in Pharmaceutical Formulation by an Optimized Novel Luminescence Method Using CdS Quantum Dots as Sensitizer

In this article, a novel chemiluminescence method using water-soluble CdS quantum dots (QDs) as sensitizers is proposed for the chemiluminometric determination of epinephrine. The method is based on the quenching effect of epinephrine on the chemiluminescence emission generated by the mixing of CdS quantum dots (QDs) with hydrogen carbonate (HCO₃ ^-) in the presence of hydrogen peroxide (H₂O₂) in an alkaline medium. The optimization of variables influencing the chemiluminescence response of the method has been carried out by using experimental design. Under the optimal conditions, there is good linear relationship between the relative chemiluminescence intensity and the concentration of epinephrine over the range of 5?×?10^?9–1?×?10^?6?molL^?1 with a 3σ detection limit of 5?×?10^?11?molL^?1. The method has been successfully applied to the determination of epinephrine in pharmaceutical formulation and the recovery test was done in human urine.     

Binding Study of Phenformin with Bovine Serum Album Using a Combined Technique of Equilibrium Dialysis with Flow-Injection Chemiluminescence Detection

ABSTRACT

The interaction between phenformin hydrochloride and bovine serum albumin (BSA) was investigated by the methods of chemiluminescence combined with equilibrium dialysis technique. A novel N-bromosuccinimide (NBS)–eosin Y (EY) chemiluminescence (CL) method was established for the determination of phenformin. The mechanism of this chemiluminescence system was proposed. Optimization studies were performed to determine the phenformin. Under the optimal conditions, the CL intensity was linear for a phenformin concentration over the range of 4.6 × 10^?8 to 5.0 × 10^?5 g/mL. The detection limit was 1.5 × 10^?8 g/mL. The data obtained by the present equilibrium dialysis–CL system were analyzed using the Klotz plot and the Scatchard analysis. The results showed that the Klotz plot and the Scatchard plot are linear with good correlation coefficient, indicating that the phenformin has only one type of binding site on BSA. The binding parameters were the number of the binding sites n (1.02) and the estimated association constant K (2.66 × 10⁴ L/mol). The chemiluminescence system combined with equilibrium dialysis developed in this work demonstrated its use for determination of interaction between drug and protein by using relatively simple instrument.     

Determination of iodide in urine based on chemiluminescence system of cerium (IV)–tween 40–iodide

In acidic medium, the oxidation reaction of cerium (IV) with iodide can produce strong chemiluminescence (CL) in the presence of surfactant tween 40 as an enhancer. On this basis, a flow injection method with CL detection was established for the determination of iodide. The method is simple, rapid and effective to determine iodide in the range of 8.0×10^?8–5.0×10^?5 mol/L with a determination limit of 5.0×10^?8 mol/L. The relative standard deviation is 2.7% for the determination of 5.0×10^?6 mol/L iodide (n=11). The method has been applied to determine the content of iodide in urine with satisfactory results. Furthermore, it is suggested that the light emission from cerium (IV)–tween 40 reaction is probably because of the formation of singlet oxygen ¹O₂^? and the emitter is excited oxygen molecular pairs O₂(¹Δ_g)O₂(¹∑_g^?).