Liquid chromatographic purification and detection of anabolic compounds.

The role of liquid chromatography within methods of analysis for steroids, related compounds and beta-agonists in biological samples is discussed. Special attention is given to the application of liquid chromatography in sample preparation and extract clean-up. Different forms of liquid chromatography, including immunoaffinity chromatography, are compared and evaluated. Methods for confirmation based on gas chromatography-mass spectrometry and cryotrapping Fourier transform infrared spectrometry are discussed.     

饮用水中有机污染物检测方法研究进展

介绍水中有机污染物的富集方法如顶空法、萃取法、固相微萃取法、液相微萃取法、棒吸附萃取等,对饮用水中有机污染物的检测技术如气相色谱法、气相色谱–质谱联用法、液相色谱法、液相色谱–质联用法等进行了综述并对检测技术的发展趋势进行了展望。     

Capillary electrophoresis and capillary electrochromatography of organic pollutants

Capillary electrophoresis (CE) has a unique capability for separation of analytes of environmental concern, particularly those that are more polar and ionic, based on the complementary separation principle of electrophoresis. In the past few years, CE has been selectively used to analyze various classes of compounds having current or potential environmental relevance. This review outlines the current status of CE for the determination of environmental pollutants, based predominantly on research results published from the beginning of 1997 to early 1999. Covered are environmental pollutants of all types except pesticides and inorganics. Certain naturally produced toxins are also covered because of their significant impacts upon human health and the environment. CE methods, as with all methods, must be judged on their ability to provide approaches that are reliable, sensitive, selective, and rapid, while meeting "green chemistry" initiatives for pollution prevention. We also compare CE methods to benchmark environmental techniques involving gas chromatography-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (LC-MS), and high performance liquid chromatography (HPLC).     

类固醇兴奋剂分析方法的研究进展

蛋白同化雄性类固醇是一类滥用最为普遍的兴奋剂物质,对其进行有效的控制和检测关系到运动员的身心健康和体育比赛的公平公正。对类固醇兴奋剂分析方法的改进和发展是目前兴奋剂检测的重要任务。本文主要是对自2002年以来类固醇兴奋剂样品的预处理和检测手段的研究进展做一概述,包括气相色谱-质谱法、液相色谱-质谱法、免疫法、电化学方法以及质谱法等。     

质谱分析技术在纺织品检测方面的应用

介绍纺织品中有害物质标准检测方法中质谱分析技术的应用,概述了气相色谱-质谱联用、高效液相色谱-质谱联用和电感耦合等离子体-质谱联用技术在纺织品检测方面的广泛应用及其发展前景.     

色谱-质谱联用技术在代谢组学中的应用

代谢组学是对生物体受外部刺激所产生的小分子代谢产物的变化或其随时间的变化进行研究的一门学科,以实现对体液、细胞以及组织提取物等复杂的生物样本中所有代谢产物的定性和定量分析为研究目标。色谱-质谱联用技术在代谢组学的研究中已显示出极大的发展潜力。本文主要综述近年来代谢组学研究中涉及的色谱-质谱联用技术及其数据处理方法,重点介绍各种分离技术的特点及其在应用中的关键问题,并对其在代谢组学应用中的未来发展给予展望。     

Methods for the determination of sulphonamides in meat.

Sulphonamides, due to their important antibacterial effects, are widely used in veterinary practice and animal husbandry. Residues arising from administration without observing withdrawal time sufficiently are normally the parent compounds and the N4-acetyl derivatives, the latter being hydrolyzed to the parent compounds only during extraction under acidic conditions. It is therefore quite conceivable that many authors concentrate on determining these metabolites. In the past decade, we have witnessed a considerable increase in new analytical techniques dealing with the determination of sulphonamides. Among these procedures, especially the so-called multimethods using high-performance liquid chromatography--though sometimes including toilsome clean-up steps--can be mentioned. However, current approaches also utilize gas chromatography, gas chromatography-mass spectrometry, liquid chromatography-mass spectrometry, supercritical fluid chromatography-mass spectrometry, thin-layer chromatography and immunological methods. For most of these techniques, a strong trend towards lowering the level of detectability (down to the sub-ppb range) and improving accuracy and reproducibility can be established.     

Properties of the Adsorption Equilibrium Isotherms Used and Measured in RPLC

Monitoring anabolic steroids in meat-producing animals is a challenging task. It implies very specific and sensitive analytical methods able to detect and identify sub-μg kg^?1 residue levels in complex biological matrices such as meat, urine, or hair. Gas and liquid chromatography coupled to mass spectrometry are the most efficient means of achieving these objectives. In this paper we review how developments in mass spectrometry have been rapidly applied to this problem, how efficient analysis of anabolic steroids in urine, edible tissue, and hair has been achieved, and, later, how measurement of conjugate steroids and determination of the origin of natural steroid hormones has been achieved. The performance characteristics of different mass spectrometers (quadrupole, ion-trap, electromagnetic, isotope-ratio, tandem, and hybrid instruments), the efficiency of different acquisition techniques (LR-SIM, HR-SIM, MRM), and, finally, sample introduction (gas chromatography and liquid chromatography, with discussion of alternative interfaces) are discussed, with numerous applications.     

Application of liquid chromatography coupled with electrospray ionization time-of-flight mass spectrometry for screening and quantitative analysis of C21 steroids in the roots and rhizomes of Cynanchum paniculatum

A liquid chromatography-mass spectrometry method is presented for the quantification of C21 steroids in the roots and rhizomes of Cynanchum paniculatum. Eight C21 steroids, including five steroidal aglycones and three steroidal glycosides, were simultaneously analyzed by liquid chromatography coupled with electrospray ionization time-of-flight mass spectrometry. The extracted ion current chromatograms were extracted from the total ion current chromatogram using characteristic ions produced by target compounds for peak determination. Chromatographic separation was achieved on a C18 reversed-phase column within 60 min, using an acetonitrile/water gradient. For comparision, six C. paniculatum samples from different locations were investigated by the established method, and the results indicated that the different geographical origin significantly influenced the C21 steroid composition. The method was observed to have the necessary sensitivity, selectivity, precision, and accuracy, and to be suitable for quality control of herbal medicines and their preparations.     

褪黑素含量测定方法

褪黑素因对人体具有一定的保健功能而作为保健品的主要添加成分被广泛使用。测定褪黑素含量的方法有生化免疫方法、紫外分光光度法、色谱法及色谱-质谱联用法等。主要介绍用气相色谱-质谱联用法、紫外分光光度法和高效液相色谱法测定褪黑素的含量。     

水体中硝基芳烃类有机污染物分析方法研究进展

硝基芳烃类有机物是一类重要的化工原料,也是性质相对稳定、难以降解的高毒污染物。其检测技术主要有分光光度法、电化学法、液相色谱法、气相色谱-电子捕获检测器法(GC/ECD)、气相色谱-质谱法(GC-MS)等。其中GC/ECD法和GC-MS法因测定准确、灵敏、适用范围广而得到广泛应用。该文从不同类型水体中硝基芳烃类有机物样品的采集、前处理以及检测分析技术的选择角度,对硝基芳烃类有机物检测技术的发展进行了简要评述,同时对其分析方法进行了展望。     

Analytical tools for urocanic acid determination in human samples: A review

Urocanic acid is a chromophore found in the skin that has been identified as an important immunosuppressant and carcinogenesis mediator through its photoisomerization from trans to cis form induced by ultraviolet radiation. Research on analytical methods that explore urocanic acid isomerization is indispensable to fully understand the deleterious effects mediated by this biomarker. In this context, the current relevant analytical methods for determination of these isomers in human samples are summarized in this review. The methods presented here are applicable to human samples collected by noninvasive methods (or minimally invasive), encompassing an array of analytical techniques, including high‐performance capillary electrophoresis, confocal Raman spectroscopy, gas chromatography, high‐performance liquid chromatography, and mass spectrometry, among others. Developed high‐performance liquid chromatography methods have proven to be advantageous, allowing noninvasive collections for in vivo analysis and the confocal Raman, specially, for real‐time analysis. Among all these methods, high‐performance liquid chromatography is the most investigated one with mass spectrometry or ultraviolet detector, and the mass spectrometry detector being the most studied in the last years, demonstrating high sensitivity, very low detection limits, and accurate identification, especially for clinical investigations.     

Mit Chromatographie und Spektrometer: Forensische Toxikologie

Toxicology is a classic field of forensic medicine. Forensic toxicology includes the analysis of medical and illegal drugs and dangerous substances in order of courts, investigating authorities and hospitals. Fast and easy immunological techniques for assying drug familys or single drugs are available. The conventional methods for detection of drugs are generally instrumental procedures such as gas chromatography, high‐performance liquid chromatography and chromatography‐mass spectrometry.     

Multi-dimensional chromatography using on-line coupled microcolumn liquid chromatography—capillary gas chromatography for quantitative pesticide residue analysis

Highly selective separations can be achieved by utilizing different separation modes in a multi-dimensional (on-line coupled) chromatographic system. The application of such a system utilizing microcolumn liquid chromatography coupled on-line to capillary gas chromatography for the determination of 2-(1,1-dimethylethyl)-5-pyrimidinol, a pesticide metabolite, in various corn matrices at the ng g^?1 level is described. A comparative quantitative study with conventional manual sample pretreatments followed by capillary gas chromatography-mass spectrometry indicated equivalence between the two techniques. The system offers the advantages of reduced sample handling steps and analysis time, high potential for automation and adequate sensitivity.     

PRODUCTS OF CHLOROPHYLL PHOTODEGRADATION–2. STRUCTURAL IDENTIFICATION

Abstract— Hydrophilic products of chlorophyll a photodegradation are structurally identified using UV/visible and fourier transform infrared spectrophotometry and gas chromatography-mass spectrometry. The major peak detected during reverse-phase high performance liquid chromatography of the colourless photodegradation products is identified as glycerol. Lactic, citric, succinic and malonic acids, as well as alanine, are also identified.     

A fast, comprehensive screening method for doping agents in urine by gas chromatography-triple quadrupole mass spectrometry

The use of performance enhancing drugs in sports is prohibited. For the detection of misuse of such substances gas chromatography or liquid chromatography coupled to mass spectrometry are the most frequently used detection techniques. In this work the development and validation of a fast gas chromatography tandem mass spectrometric method for the detection of a wide range of doping agents is described. The method can determine 13 endogenous steroids (the steroid profile), 19-norandrosterone, salbutamol and 11-nor-Δ9-tetrahydrocannabinol.9carboxylic acid in the applicable ranges and to detect qualitatively over 140 substances in accordance with the minimum required performance levels of the World Anti-Doping Agency in 1ml of urine. The classes of substances included in the method are anabolic steroids, β2-agonists, stimulants, narcotics, hormone antagonists and modulators and beta-blockers. Moreover, using a short capillary column and hydrogen as a carrier gas the run time of the method is less than 8min.     

Determination of nalbuphine using high-performance liquid chromatography coupled to photodiode-array detection and gas chromatography coupled to mass spectrometry.

A procedure involving capillary column gas chromatography coupled to mass spectrometry and a method involving liquid chromatography coupled to a diode-array detector have been developed for the analysis of nalbuphine. The extraction step is the same for both techniques and involves extraction under alkaline conditions in chloroform-2-propanol-n-heptane (50:17:33, v/v/v) with levallorphan as the internal standard. After purification by acidic extraction and back alkaline extraction, drugs are derivatized with N,O-bis-(trimethylsilyl)trifluoroacetamide with 1% trimethylchlorosilane for gas chromatography-mass spectrometry and directly injected for high-performance liquid chromatography-diode-array detection. The limits of detection are 2.0 and 25.0 ng/mg, respectively.     

Application of analytical chemistry in the quality evaluation of Glycyrrhiza Spp

Licorice, one of the oldest traditional Chinese medications, is widely used in the treatment of various diseases. With the development of science and technology, an increasing amount of analytical techniques have been applied to the quality control of licorice. Herein, we summarize several of the quality control methods developed in recent years. These approaches include sample preparation processes, high-performance thin layer chromatography, gas chromatography, gas chromatography/mass spectrometry, high-performance liquid chromatography, and liquid chromatography/mass spectrometry (LC/MS). Among these various techniques, LC/MS has come forward as one of the main methods forquality control of licorice.     

Ceramide analysis utilizing gas chromatography-mass spectrometry

Suitable analytical methods are a prerequisite of a detailed investigation of ceramides. Therefore, a new gas chromatograph-mass spectrometry method with electron impact ionization was developed. Samples have been prepared for gas chromatography by the formation of volatile trimethylsilyl derivatives. The method provides high separation efficiency, sensitivity and specificity. Mass spectra facilitate the structural characterization of each species, because certain fragments indicate the fatty acid as well as the sphingoid base moiety. In a 30-mm run even very similar ceramides are baseline separated. The method is compared to a recently published assay for liquid chromatography-mass spectrometry.     

高效液相色谱及液相色谱-质谱联用技术在保健食品检测中的应用

综述了近年来高效液相色谱和液相色谱-质谱联用技术在保健食品检测中的应用。这些应用包括保健食品中维生素、多不饱和脂肪酸、类胡萝卜素、多糖类、皂甙类和黄酮类营养物质的测定。