环境内分泌干扰物分析方法的研究与进展

本文对近5年来国内外环境内分泌干扰物的研究进展进行了综述,包括环境内分泌干扰物的分类、样品前处理技术、检测技术等,并对环境内分泌干扰物分析的发展进行了总结和展望,引用文献286篇。     

我国环境中有机污染物分析方法及痕量富集技术的进展

对有机污染物分析在近年进展作了评述。其主要内容涉及试样的预处理技术（如顶空法,吹扫-捕集法,固相萃取,半透膜等技术）,各化合物的适用及有效的分析方法或仪器（如GC,HPLC及GC／MS等）以及各种技术及方法的联用技术等（引述文献37篇）。     

多类环境内分泌干扰物高效共同测定项目总结报告

环境中的内分泌干扰物质种类多样、浓度低且来源广、危害大,对环境中的内分泌干扰物进行及时准确检测,能有预防环境中的内分泌干扰物造成的危害,是对内分泌干扰物进行预防和治理的关键步骤。     

环境样品中硝基苯类化合物的分析方法研究进展

主要介绍了我国近年来在环境样品中硝基苯类化合物的分析研究进展,内容包括:光度法(还原-偶氮光度法、阻抑动力学光度法、化学计量学分光光度法、人工神经网络-分光光度法)、气相色谱法(固相微萃取-毛细管气相色谱法、树脂吸附-气相色谱法、液-液微萃取气相色谱法、超声萃取-气相色谱法)、高效液相色谱法(反相高效液相色谱法、固相萃取-高效液相色谱法)和极谱法等分析方法。     

环境和生物样品中铂族金属的分析研究进展

评述了近年来环境和生物样品中痕量铂族金属的分析研究进展，重点介绍了样品的预处理和分离富集技术以及检测手段等。     

香精香料的分析方法进展

本文对香精香料的前处理、分离和检测方法的研究进展进行了综述。对一些新的分析方法作了简要介绍。引用文献34篇。     

地质环境样品中挥发酚分析现状与进展

挥发酚被列为环境优先控制的有机污染物,已成为评价环境污染的重要指标之一。该文简述了挥发酚的化学性质及地质环境来源,概括了国内外挥发酚测定的相关标准方法,从样品预处理技术和检测技术两方面综述了近年来地质环境样品中挥发酚分析的研究现状。重点对溶剂萃取、蒸馏、固相萃取、固相微萃取和吹扫捕集等样品预处理技术,以及4-氨基安替比林分光光度法、紫外和荧光分光光度法、溴化容量法、气相色谱法、液相色谱法和酚生物传感器法等技术在地质环境样品中挥发酚分析上的应用进行了较为全面的总结,并对其未来的发展趋势进行了展望,为进一步研究挥发酚的分析技术及其环境应用提供参考。     

水环境中微塑料的样品采集与分析进展

微塑料在环境中难以降解,可在水体、沉积物等环境介质中长期存在,并在水生生物体内积累,成为人们高度关注的环境问题之一。有关水环境中微塑料的污染研究尚处于起步阶段,快速、高效、准确的检测技术是水环境中微塑料研究的重要环节,对于优化研究路线、分析研究结果、总结微塑料污染规律至关重要。本文结合国内外微塑料污染研究进展,介绍了微塑料污染现状,并通过对环境样品中微塑料的采样、预处理以及定性定量分析方法的系统比较,总结了现行各种检测方法的优缺点及各自应用范围,最后指出了进一步研究的方向。     

纳米塑料分析方法研究进展

对近十年纳米塑料的分析方法进行综述.分别总结了样品消解、滤膜过滤、浊点萃取、加压流体萃取等纳米塑料的预处理方法,介绍了热解–气相色谱–质谱联用、热吸附解析–气相色谱–质谱、热脱附–质子转移反应–质谱、液相色谱–质谱/质谱联用、热重分析–质谱等分析方法,并对方法的优缺点进行分析.展望了未来纳米塑料分析方法的发展,该研究为...     

蝶呤类化合物分析方法研究进展

本文概述了国内外蝶呤类化合物分析方法的研究现状,包括高效液相色谱法、荧光分析法、免疫分析法、毛细管电泳法等,同时对人体的尿液和血液等样品的前处理方法进行了介绍。引用文献49篇。     

Determination of Endocrine Disruptors in Environmental Water by Single-Drop Microextraction and High-Performance Liquid Chromatography

Using single-drop microextraction followed by high performance liquid chromatography, an effective method for the rapid extraction for endocrine disruptors, including estrogens and alkylphenols, was developed. Factors that influenced the extraction efficiency, such as hydrogen bonding, hydrophobic property, polarity, and van der Waals forces, were evaluated in detail. The results indicated that bisphenol A and estrogens were extracted effectively by the solvents with hydrogen bond acceptors and higher polarity; alkylphenols preferred solvents that could supply strong van der Waals forces or possessed π-π stacking structures and superior hydrophobicity. The optimum extraction conditions were determined, including extraction time, pH, and salt effects. Under the optimized conditions, high extraction factors (≥147) were achieved. Limits of detection for the endocrine disruptors were between 0.33 and 0.67 µg L^?1. The method strategy is well suited for the determination of trace levels of endocrine disruptors in environmental water.     

The Voltammetry and Electroanalysis of Some Estrogenic Compounds at Modified Diamond Electrodes

The voltammetry of some estrogenic compounds (estradiol, nonylphenol, bisphenol A, ethynylestradiol, estrone, estriol) in aqueous solution at boron doped diamond electrodes is reported. For oxidised (hydrophilic) electrodes electrochemically irreversible kinetics were observed for the diffusing molecules allowing the inference of diffusion coefficients and transfer coefficients. In contrast for hydrogen terminated (hydrophobic) surfaces significant adsorption was observed. A limit of detection of 1–100 µM for the estrogenic compounds was found using the oxidised diamond electrode. Surface modification of the oxidised diamond with nano‐Carbon (so‐called Carbon Black) allowed preconcentration of the target by adsorption onto the Carbon Black prior to analysis and a corresponding reduction of the limit of detection by ca three orders of magnitude to 5–100 nM.     

农、兽药及工业化学物残留量分析中样品前处理微量化学法技术研究

建立了一种用于残留物分析样品处理的微量化学法(MICCM)体系,提出了该体系的基本概念、原理、单元操作,选择了一套基本系列设备和器具,并将这一体系用于检测不同样品中的农药、兽药、工业化学物残留量及食品添加剂。实例中,各方法检测限、回收率、变异系数的实验数据均达到了国际上对残留量分析方法的技术要求。该体系与经典常量化学法(MaCCM)样品处理体系相比,具有快速、简便、工效高,节省人力、试剂材料、能源以及占用场地小等多种优点。残留物分析可广泛用该体系取代经典法样品处理体系。     

Development of a fabric phase sorptive extraction with high‐performance liquid chromatography and ultraviolet detection method for the analysis of alkyl phenols in environmental samples

A novel analytical method has been developed and validated for the quantification of alkyl phenols in aqueous and soil samples. Fabric phase sorptive extraction, a new sorptive microextraction technique, has been employed for the preconcentration of some endocrine‐disruptor alkylphenol molecules, namely, 4‐tert‐butylphenol, 4‐sec‐butylphenol, 4‐tert‐amylphenol, and 4‐cumylphenol, followed by high‐performance liquid chromatography with ultraviolet detection. Various parameters influencing the fabric phase sorptive extraction performance, namely, extraction time, eluting solvent, elution time and pH of the sample matrix, were optimized. The chromatographic separation was carried out with a mobile phase of acetonitrile/water (60:40 v/v) at an isocratic flow rate of 1.0 mL/min using a reversed‐phase C₁₈ column at λ_max 225 nm. The calibration curves of target analytes were prepared in the concentration range 5–500 ng/mL with good coefficient of determination values (R² > 0.992). Extraction efficiency values were 74.0, 75.6, 78.0, and 78.3 for 4‐tert‐butylphenol, 4‐sec‐butylphenol, 4‐tert‐amylphenol, and 4‐cumylphenol, respectively. The limits of detection range from 0.161 to 0.192 ng/mL. Subsequently, the new fabric phase sorptive extraction with high‐performance liquid chromatography and ultraviolet detection was successfully applied for the recovery of alkyl phenols from spiked ground water, river water, and treated water from a sewage treatment plant, and soil and sludge samples.     

Automation of sample preparation as a preliminary stage in the high-performance liquid chromatographic determination of polyphenolic compounds in sherry wines

The procedure for automating the method of sample preparation by solid-phase extraction prior to the HPLC analysis of polyphenolic compounds in sherry wine is described. This method consists of two stages, the first being sample preconcentration and cleaning using a C₁₈ cartridge and the second fractionation using a SAX anion exchanger. The first direct application of the method, using a semi-flexible robot system, did not produce satisfactory results, thus requiring a series of modifications and optimization of the variables inherent in the device itself. The automated method as modified produced considerable improvements over the manual method with respect to the recovery and repeatability values obtained with the different polyphenolic species used in its optimization. Subsequent testing of the method with real samples of sherry wine proved its applicability for tracking the evolution of polyphenolic species in wine.     

兴奋剂中利尿剂的检测方法

利尿剂是国际奥委会医学委员会禁止使用的一类兴奋剂。该文对兴奋剂中利尿剂的检测方法进行了综述,重点阐述了样品的处理方法,HPLC－GC－MS的检测方法及各种衍生化方法。     

Solventless Sample Preparation Techniques in Environmental Analysis

This review focuses on the role of so‐called solventless methods of sample preparation in contemporary environmental analysis. The basic classification of this group of methods as well as the principal features and advantages of the techniques in current use are discussed.     

Analysis and Speciation of Traces of Arsenic in Environmental,Food and Industrial Samples by Voltammetry: a Review

Voltammetric approaches for the determination of arsenic and speciation at trace levels are critically appraised in a review covering the literature from 1970 to 2002. Special attention is devoted to stripping modes and to issues related to the choice of working material and supporting electrolyte. A section is dedicated to the management of real samples and aspects of sample preparation. An extensive compilation, organized by real sample type, gathers essential experimental conditions. Potentiometric stripping analysis is introduced for sake of comparison. The coupling of voltammetric detection or preaccumulation with FIA, chromatography, capillary electrophoresis and ICP techniques is also addressed.     

Organomercury Compounds. 32. Syntheses of Fluorophenylmercurials by Decarboxylation

The organomercury compounds HgR₂ (R = 2-Cl,6-FC₆H₃, 2,6-F₂C₆H₃, 2,3,6-F₃C₆H₂, m-HC₆F₄, p-HC₆F₄, or C₆F₅) and RHg(O₂CR) (R = 2-Cl,6-C₆H₃, 2,6-F₂C₆H₃ or 2,3,6-F₃C₆H₂) have been obtained in moderate – good and low yields respectively from decarboxylation reactions of the corresponding mercury(II) fluorobenzoates in boiling pyridine. By contrast, mercury(II) 2,3,4-5-tetrafluorobenzoate gave a low yield of CO₂, a trace of Hg(o-HC₆F₄)₂ and a very low yield of o-HC₆F₄Hg(O₂CC₆F₄H-o). The ¹⁹⁹Hg NMR spectra of the diorganomercurials (R = 2-Cl,6-FC₆H₃, 2,6-F₂C₆H₃, 2,3,6-F₃C₆H₂, 2,4,6-F₃C₆H₂, 2,6-Cl₂C₆H₃, o-HC₆F₄, m-HC₆F₄, p-HC₆F₄ or C₆F₅) are discussed.     

用偏最小二乘法—荧光光谱法定量分析芳烃混合物

本文用偏最小二乘法方法来解析荧光的激发发射和左阵，直接定量分析荧光混合物试样。文中分析了ＥＥＭ的特点，介绍了用ＥＥＭ－ＰＬＳ定量分析试样的思路和方法，并对５个模拟混合物和４个实际混合物进行了测试和计算，获得了满意的结果。本文还用实例讨论了数据中的异常点，对结果的影响及晚年剔除的方法。