化学发光技术在色谱柱后检测中的应用

化学发光与色谱联用具有选择性好、灵敏度高等优点,应用广泛.本文主要介绍近三年来化学发光包括鲁米诺、过氧草酸酯、Ru(bipy)33 、无机等体系作为液相色谱柱后检测及含氮、含硫化合物气相化学发光等体系作为气相色谱柱后检测的现状.     

高效液相色谱-化学发光法检测牛奶中磺胺类药物残留

以4种磺胺类药物(Sulfonamides, SAs), 即磺胺脒(Sulfaguanidine, SGD)、磺胺嘧啶(sulfadiazine, SDZ)、磺胺噻唑(sulfathiazole, STZ)和磺胺二甲嘧啶(Sulfamethazine,SMZ)为分析物,基于其在碱性介质中对Ag配合物-鲁米诺(Luminol)与Ni配合物鲁米诺两化学发光体系发光强度均具有抑制作用的性质,建立了高效液相色谱-化学发光法检测牛奶中4种磺胺类药物的方法.将化学发光体系作为高效液相色谱的新型检测器,并对两种化学发光体系的检测器性能进行了比较.4种磺胺药物经高效液相色谱分离后,分别与Ag-Luminol及Ni-Luminol化学发光体系作用.色谱条件为:反相C18分离柱(250 mm × 4.6 mm,5 μm);0.1%甲酸-甲醇为流动相(V/V);梯度洗脱;流速1 mL/min.化学发光条件:Ag、Ni-Luminol两体系中,Ag配合物浓度1.4×10.-4 mol/L(含0.12 mol/L NaOH);Ni配合物浓度1.5×10.-5 mol/L(含0.12 mol/L NaOH);Luminol浓度均为1.2×10.-7 mol/L;试剂流速均为1.0 mL/min.在最佳的分离检测条件下,Ag-Luminol体系检测4种磺胺类药物的检出限分别为0.15、0.96、1.10和1.50 μg/mL,加标回收率为81.0%~101.5%;Ni-Luminol体系检测SGD、SDZ、STZ 3种磺胺类药物的检出限分别为1.5、17.2和16.8 μg/mL,加标回收率为83.9%~110.8%.相比之下,Ag-Luminol体系作为高效液相色谱检测器更佳.应用本方法对牛奶中4种磺胺类药物残留量进行检测,结果令人满意.     

有机化合物的化学发光分析

本文综述了化学发光反应测定有机化合物的几种主要类型,简单介绍了液相化学发光反应在环境保护、临床医学、制药工业,农药、有机合成、微生物以及薄层色谱、高效液相色谱方面的分析应用。     

现代分析检测技术在润滑油氧化中的应用

介绍了近20年来用于润滑油氧化测试中分析检测技术的进展情况,包括高效液相色谱、气相色谱、凝胶渗透色谱、热分析、红外光谱、核磁共振、化学发光及电化学技术,并讨论了今后发展的方向。     

流动注射化学发光检测法的进展

评述近年来流动注射化学发光检测法及生物发光检测法的最新进展。内容涉及各类化学发光反应、生物发光和电致化学发光反应同流主射体系的耦合方式，仪器设计，多种无机、有机、生物大分子、生物活性的药物的分析方法及其在环境、生物医学客生命科学、化学及药物化学中的应用和发展方向。     

化学发光在生化分析中的应用研究进展

化学发光分析是利用化学发光反应的发光现象,对化学发光物质由激发态跃迁回基态时发出的光信号进行测量的一种分析方法。化学发光分析具有无需外来光源、灵敏度高、操作方便、分析快速以及易于实现自动化等优点,可与其它分析技术联用,在临床检验、药物分析和环境监测等领域具有广泛应用。近年来,纳米材料、生物芯片及微流控技术的引入促进了化学发光分析技术的发展。本文综述了化学发光分析与高效液相色谱、毛细管电泳、量子点、微流控芯片和微阵列、以及滚环扩增、等温指数扩增和两级等温扩增联用技术的发展,介绍了化学发光分析技术在DNA、生物小分子、生物酶、蛋白质和金属离子检测中的应用研究进展,并展望了其发展趋势。     

苯二酚异构体的高效液相色谱化学发光检测法研究

高效液相色谱作为一种有效的分离手段已被用于酚类化合物的分析 ,紫外检测法 [1～ 3] 、电化学检测法[3,4 ] 等已用于苯二酚异构体的测定 ,但苯二酚异构体的化学发光检测法尚未见文献报道 .前文 [5] 结果表明 ,苯二酚异构体等对鲁米诺诱导的化学发光具有很强的抑制作用 .基于此 ,本文将高效液相色谱与化学发光技术联用 ,首次建立了苯二酚异构体的高效液相色谱化学发光检测法 .该法灵敏度高 ,选择性好 ,为酚类物质的测定提供了一条新的途径 .1　实验部分1 .1　仪器与试剂　 FIA- 2 4 0 0型流动注射分析仪 (中国科学院信通科学仪器公司 ) ;G…     

液相色谱化学发光检测法的新进展

本文评述了近年来液相色谱化学发光检测法的新进展，内容涉及各类化学发光发反应，生物发光反应和电致化学发光反应同色谱体系的偶合方式，仪器设计，多种无机，有机，生物大分子和生物活性物质的分析方法及其在环境，生物医学科学和生命科学中的应用和发展方向。引用文献１６８篇。     

高效液相色谱在生物医药研究中的应用 第一讲 高效液相色谱在植物化学中的应用

中国科学院上海药物研究所张仁斌等编写的《高效液相色谱在医学研究中应用》一书曾受到广大色谱工作者的欢迎,该书出版后不久即销售一空,不少读者来信希望再版,出版社和有关作者认为与迅速发展的色谱学科相比,该书内容显得陈旧,再版意义不大。在色谱杂志编委的倡议和支持下,我们组织了中国科学院上海药物研究所及兰州化学物理研究所有关学科的科研人员,根据近年来色谱在这方面的新进展和自身的实践经验,编写了“高效液相色谱在生物医药研究中的应用”系列讲座,在色谱杂志上刊登,供从事这方面工作的同志参考。由于高效液相色谱技术发展很快,我们在编写中难免有不足之处,欢迎读者提出宝贵意见和建议。     

分子印迹技术在化学发光分析中的应用

分子印迹技术具有预定性、识别性和实用性的特点,因此在化学催化、材料科学、色谱分离、仿生传感等方面得到了广泛的应用.该文概述了分子印迹技术的研究进展,综述了分子印迹技术在化学发光分析中的应用进展,包括化学发光传感器及固相萃取-化学发光应用研究.     

Flow-Based Methods with Chemiluminescence Detection for Food and Environmental Analysis: A Review

This paper presents an overview of flow-based methods in food and environmental analysis using chemiluminescence (CL) detection covering the period from 2005 to the present. The review discussses both automated flow methods of analysis [such as flow-injection analysis (FIA), sequential-injection analysis (SIA) and their variants] and separation techniques [liquid chromatography (LC) and capillary electrophoresis (CE) coupled to CL detection]. The most widely used CL reactions are presented together with representative applications in food and environmental analysis (determination of naturally occurring compounds, contaminants, additives as well as determination of inorganic and organic compounds).     

Procedures for the enhancement of selectivity in liquid phase chemiluminescence detection

An overview of liquid phase chemiluminescence (CL) processes is presented and the potential for CL detection in liquid chromatography (LC) is discussed, with particular reference to the luminol and peroxyoxalate reactions. Post column ion displacement from a solid phase reagent [a cation exchange resin in the copper(II) form] followed by catalysis of the luminol reaction is used for the quantification of mixtures of weak acids after separation by ion-exclusion chromatography. Polyaromatic hydrocarbons (PAHs) released during the combustion of biomass fuels are separated by reversed-phase chromatography and quantified by their sensitizing effect on the peroxyoxalate reaction. This procedure is also used for the determination of carboxylic acids in non-aqueous media after selective pre-column derivatization with a fluorescent label (9-anthracenemethanol).     

Chromatographic determinations of a beta-lactam antibiotic, cefaclor by means of fluorescence, chemiluminescence and mass spectrometry

We report analytical informations on the quantification of cefaclor (CCL), a beta-lactam antibiotic by three detection methods. The methods were based on the chemical derivatization of the drug with 4-(2'-cyanoisoindolyl)phenylisothiocyanate (CIPIC) under the reaction conditions with heating at 80 degrees C for 7 min in the presence of pyridine. The CIPIC reagent could react with the primary amino group of the drug to form CIPIC-conjugated CCL. The derivative emitted not only fluorescence (FL) at maximum emission wavelength of 410 nm with the irradiation at 310 nm excitation, but also chemiluminescence (CL) in the presence of H(2)O(2), borate buffer (pH 9.5) and acetonitrile. After reversed-phase liquid chromatographic separation of the CIPIC-conjugated CCL in blood, the derivative could be monitored with a FL detector, indicating the detection limit (S/N=3) of 10 pmol/injection. The CIPIC-conjugated CCL was further monitored most sensitively by a CL detector after simply mixing H(2)O(2) and borate buffer with the column eluate. The CL detection limit was 1.0 pmol/injection. In addition, we attempted to detect the CIPIC-conjugated CCL by liquid chromatographic-mass spectrometry (LC/MS). The MS method permitted the specific detection of the CIPIC derivative of the drug, though the sensitivity was 10(4)-times lower than that of the CL detection.     

A novel chemiluminescence technique for quantitative measurement of low concentration human serum albumin.

An efficient and highly sensitive chemiluminescence (CL) technique is proposed in the current study for detection of low levels of human serum albumin (HSA). Chemiluminescence (CL) produced during interaction between fluoresceinyl cypridina luciferin analog (FCLA)-1O2 can be modified with the presence of HSA. The conventional CL technique uses a quenching effect of HSA for its quantitative measurement. We are reporting here that the CL intensity can be enhanced, rather than quenched, by the addition of HSA. The CL signal can be linearly correlated with the HSA concentration over a clinically interesting range of 5 x 10(-9) - 8 x 10(-8) mol L(-1), with a detection limit of 2.5 x 10(-9) mol L(-1). The determination result was consistent with that obtained from conventional methods. One possible mechanism of HSA detection technique using CL enhancement approach is discussed. Intermolecular energy transfer in chemiluminescence systems and changes of microenvironment are likely to be contributors of the CL enhancement with HSA.     

Chemiluminescence detection in capillary electrophoresis using an ultra-fast co-catalyzed peroxyoxalate chemiluminescent reaction and electrokinetic reagent delivery

Summary Despite the impressive limits of detection and inherent selectivity afforded by peroxyoxalate chemiluminescence (POCL) detection, efficient coupling of POCL to capillary electrophoresis (CE) remains limited by the relatively slow kinetics of the reactions that drive imidazole-catalyzed chemiluminescence. Moreover, oxalate esters, used in POCL, are sparingly soluble in polar solvents and hydrolyze rapidly, presenting an additional challenge with respect to detection following aqueous phase separations. In this paper, a novel method for coupling an ultrafast POCL reaction to CE is presented. Post separation electrokinetic delivery of the POCL reagent bis(2,4,6-trichlorophenyl)oxalate (TCPO) was accomplished using a commercially available micro tee. Electrokinetic addition of TCPO allowed for precise control of the ratio of TCPO to the chemiluminescence (CL) reagents 1,2,2,6,6-pentamethylpiperidine (PMP) and 1,2,4-triazole (triazole), spiked into the running buffer. This novel method for CL reagent delivery avoided the problems and costs associated with using pressure or mechanical pumps to deliver reagents post separation. Use of this dual-component system (PMP and triazole) resulted in intense CL with half-lives of less than 2 seconds. Optimum conditions for CE-POCL detection were investigated using stopped-flow kinetics. The detection limit for 3-aminofluoranthene, following separation by CE, was<0.95 nM.     

Chemiluminescence assay for uric acid in human serum and urine using flow-injection with immobilized reagents technology

A novel chemiluminescence (CL) flow sensor for the determination of uric acid in human urine and serum has been developed by using controlled-reagent-release technology. The reagents involved in the chemiluminescence (CL) reaction, luminol and periodate, are immobilized on anion-exchange resin packed in a column. After injection of water, chemiluminescence generated by released luminol and periodate in alkaline media is inhibited in presence of uric acid. By measuring the decreased chemiluminescence (CL) intensity the uric acid is sensed. The decreased response is linear in the 5.0-500.0 ng mL(-1) range, with a detection limit of 1.8 ng mL(-1). The flow sensor showed remarkable operational stability and could be easily reused for over 80 h with sampling frequency of 100 h(-1). The proposed sensor was applied to the determination of uric acid in human urine and serum, and monitoring metabolic uric acid in human urine with RSD less than 3.0%.     

鲁米诺-铁氰化钾流动注射化学发光法测定头孢拉定

在碱性介质中,铁氰化钾氧化鲁米诺产生化学发光,头孢拉定对该体系有显著的增强作用。基于此并结合流动注射技术建立了测定头孢拉定含量的化学发光新方法。该法线性范围为0.16~160 mg/L,检出限为0.028 mg/L;对80 mg/L的头孢拉定进行平行测定11次,其相对标准偏差为0.99%。用本法对胶囊中头孢拉定进行测定,并初步探讨了该化学发光的反应机理。     

胶束微观非均相体系与化学发光能量转移

胶束微观非均相体系能提高化学发光的选择性和灵敏度,并且实验操作方便,因此其在化学发光检测技术中的应用已成为研究热点.胶束增敏化学发光是对激发量子效率,荧光量子效率以及反应的速率综合作用的结果.本文综述了正相和反相胶束体系在能量转移型化学发光体系中的应用,同时阐述了胶束与不同发光体系的相互作用.