高效液相色谱化学发光检测法测定氨基酸

本文根据铜与氨基酸组成的１：１不饱和络合物对Ｌｕｍｉｎｏｌ－Ｈ２Ｏ２化学发光体系的催化活性，设计了一种新型氨基酸高效液相色谱化学发光检测器，即在色谱柱后安装一个氢氧化铜柱，从柱后流出的氨基酸通过氢氧化铜柱时，产生配合溶解形成氨基酸－铜（１：１）络合物，进行化学发光检测，１４种常见氨基酸的检测限均在ｐｍｏｌ级，已用于血清、尿和啤酒中氨基酸的测定。     

近年国内外毛细管气相色谱柱的进展和趋向

报道了近两年毛细管气相色谱柱的发展和趋向. 气相色谱柱制柱工艺是一个成熟的技术, 所以在制柱工艺方面的研究不够活跃. 近年新研究的固定相集中在常温离子液体和各种环糊精的衍生物. 近几年GC毛细管色谱柱的研究和改进集中在色谱柱厂家进行, 并立即成为商品柱. 本文对近两年一些重要期刊上发表的气相色谱论文进行了总结, 发现气相色谱分析所用的色谱柱大都使用毛细管柱, 并趋向于使用商品GC毛细管柱, 所使用的商品色谱柱中, 使用最多的是以含5%苯基的聚甲基硅氧烷做固定相的色谱柱, 其次是以100%甲基的聚硅氧烷做固定相的色谱柱. 极性毛细管色谱柱主要使用PEG、 OV-17和OV-1701固定相.     

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.     

全二维气相色谱分析直馏柴油中含硫化合物

采用全二维气相色谱-硫化学发光检测器,以直馏柴油为研究对象,考察了一维色谱柱初始温度、升温速率及两维柱温温差等条件对含硫化合物分离的影响,建立了直馏柴油中含硫化合物的分析方法。本方法对基质复杂的直馏柴油中含硫化合物的分离,并定性分析或归类了直馏柴油中的主要含硫化合物。以苯并噻吩为测试样,以峰面积对浓度作图,硫的浓度在1～100mg/kg范围内,峰面积与硫的浓度呈线性关系,相关系数大于0.999。与传统一维气相色谱相比,全二维气相色谱技术除可检测到苯并噻吩类、二苯并噻吩类等含硫化合物外,还可检测到直馏柴油中的硫醚类化合物;苯并噻吩类和二苯并噻吩类化合物也可得到较好分离。     

多维气相色谱法检测酒中甲醇

建立了多维气相色谱检测酒中甲醇含量的方法.采用自动进样器将酒类样品直接注入气相色谱进样口,依次经过非极性RTX-5ms色谱柱和极性HP-INNOWax色谱柱,由气相色谱质谱选择离子监测技术进行测定与确证.甲醇在1～10000 mg/L范围内呈线性相关;方法检出限为1 mg/L.各种酒类样品在5,50,250,400和8...     

毛细管气相色谱法测定食品中环己基氨基磺酸钠

<正>毛细管气相色谱技术具有分离度高、重现性好和准确度高等优点,已广泛应用于各行各业的气相色谱的检测和分析中,正逐步替代填充柱色谱。但其在检测食品中环己基氨基磺酸钠时出现了标准曲线的相关性、精密度和准确度均较填充柱差的现象[1],虽然也有许多改进的方法[2-5],但无法提高测定方法的精密度和准确度,以致目前国家标准中仍以填充柱气相色谱法作为首选[6]。在用毛细管色谱     

高效液相色谱电生Mn(Ⅲ)化学发光法检测人体血清和尿样中的卡托普利

设计了一个HPLC在线电生Mn(Ⅲ)化学发光检测器, 实现在线电化学反应, 从而产生反应活性很高的初生态氧化剂Mn(Ⅲ), 并与色谱柱后CP混合产生化学发光. 同时还能够根据需要调节电极反应和发光反应两者的介质, 满足柱后发光反应的最佳环境. 在优化流动相和化学发光检测条件的基础上, 将该检测器应用于人体血清和尿液中CP的测定.     

高效液相色谱-柱后反应化学发光法检测痕量多环芳烃

过氧草酰类化学发光是六十年代发展起来的一种非酶催化高量子效率体系,量子效率高达25％。此化学发光体系已应用于色谱分离柱后反应检测荧光物质。方     

土壤中氨基酸分析方法的研究进展

本文对土壤中氨基酸的分析方法做了较详细的评述,并针对土壤氨基酸的特点,就土壤样品的前处理(主要包括水解和纯化)及目前常用的色谱分离分析方法进行了总结(主要包括柱后衍生阳离子交换色谱、气相色谱、柱前衍生反相高效液相色谱、阴离子交换色谱-积分脉冲安培检测等方法)。     

Alltech集束毛细管柱和常规毛细管柱的比较

对集束毛细管气相色谱柱的色谱性能,如流速对柱效的影响、柱温对柱效的影响、柱容量等进行了考察,并将其对典型火炸药成分ＤＮＴ,ＴＮＴ的分离与常规毛细管气相色谱柱进行了比较。结果表明,集束毛细管气相色谱柱综合了填充柱与石英毛细管气相色谱柱之优点,弥补了二者的不足,是一种柱容量较大且分离效能好、可以在高载气流速下操作的新型气相色谱柱。     

液相色谱-化学发光检测法的最新进展

评述了近年来液相色谱－化学发光检测法的最新进展,参考文献从１９９２年到１９９５年。内容涉及各类化学发光反应同液相色谱体系的耦合方式,仪器设计,多种无机、有机、生物大分子、生物活性物质及药物的分析方法及其在环境、生物医学科学和生命科学、临床化学及药物化学中的应用和发展方向。     

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。     

Hyphenated chromatographic methods for biomaterials

The improvement in hyphenated analytical techniques has significantly widened their applications to the analysis of biomaterials. In this article, we discuss recent advances in applications of hyphenated chromatographic techniques including capillary electrophoresis to the analyses of biological samples. As tools of separation, gas chromatography, high-performance liquid chromatography and capillary electrophoresis are considered with special emphasis on applications utilizing the hyphenation of these methods to mass spectrometry. Moreover, applications using other detection methods such as Fourier transform infrared spectroscopy hyphenated to gas chromatography and photodiode array detector combined with high-performance liquid chromatography or capillary electrophoresis are also discussed. Owing to their high sensitivity, luminescence-based detection systems such as laser-induced fluorescence and chemiluminescence are also included in this review.     

Ozone-based sulfur chemiluminescence detection: Its applicability to gas,supercritical fluid,and high performance liquid chromatography

The sensitive detection of sulfur-containing analytes is of interest in many industrial applications; selective detection is also desirable since these compounds are usually present at trace levels in difficult matrixes. The purpose of this article is to review the use of the Sievers® ozone-based sulfur chemiluminescence detector, and its coupling with gas chromatography, supercritical fluid chromatography, and high performance liquid chromatography. Detection limits, linearity, response factors, and selectivity are discussed for each of these techniques. Critical operational parameters for the SCD are also described. The use of other sulfur selective detectors for SFC and HPLC is also briefly summarized.     

Peroxyoxalate chemiluminescence detection with packed column supercritical fluid chromatography

Summary A detection scheme based upon peroxyoxalate chemiluminescence, which utilizes two post-column pumps and two stages of depressurization is investigated. The chemiluminescent detection limit for perylene is 23 times lower than determined by fluorescence, and is in the attomole range. This detection technique is investigated for packed column supercritical fluid chromatography (SFC). Due to the interface design used and the chemical band narrowing effects of chemiluminescence, an apparent increase in efficiency is observed. The interface design affords a wide range of pressures to be used for a separation. During pressure programming the column effluent changes flow rate. Because of a back-pressure regulator, the reaction and detection take place at nearly constant pressure. Therefore pressure gradient work is possible without concern for post-column reagent solubility (which is a concern for high-performance liquid chromatography). The effects of the expanded CO₂ from the SFC on the chemiluminescence signal and background are studied. The post-column detection is optimized for pH, photomultiplier voltage, concentrations and flow rates of the peroxide and oxalate ester.     

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).     

The use of naphthalene-2,3-dicarboxaldehyde for the analysis of primary amines using high-performance liquid chromatography and capillary electrophoresis

This paper reviews analytical methods, instrumental developments and applications for derivatization of primary amines with naphthalene-2,3-dicarboxaldehyde using fluorescence and chemiluminescence detection with capillary electrophoresis (CE) and high performance liquid chromatography (HPLC). The use of lasers as well as lamps as the excitation source for fluorescence detection is discussed. The detection limit observed with naphthalene-2,3-dicarboxaldehyde derivatization is often lower and better than those obtained with other analytical separations and other fluorescent dyes. In addition, this paper describes the crucial points that influence the stability of NDA primary amine derivatives, and summarize the separation, derivatization and migration conditions of the different techniques, with their advantages and drawbacks.     

Chemiluminescence detection in HPLC and CE for pharmaceutical and biomedical analysis

The present paper reviews the developments and applications of chemiluminescence detection with HPLC and CE in pharmaceutical and biomedical analysis. The chemiluminescence systems, chemiluminogenic reagents and derivatization reagents, improvements in instrumental design as well as their contributions to the practical applications, are all presented. The advantages and limitations of current detection methodology and future prospects for improvement are briefly discussed.     

Enzyme based detection systems in column liquid chromatography — Extension of selectivity and sensitivity

Summary Enzyme based detection systems in column liquid chromatography are described using systems based on both enzyme reactors in conjunction with a flow through detection device and enzyme electrodes. Optimizations for making detection principles compatible with chromatographic systems and applications made in our laboratories are presented for the analysis of e.g. carbohydrates, amino acids, ethanol and catecholamines. Gel-permeation chromatography and mass spectrometry are used as complementary techniques for qualitative and quantitative analysis of complex samples.