微波辅助萃取/样品前处理联用技术的研究进展

微波辅助萃取是近年来新发展的一种样品前处理技术,随着微波辅助萃取的发展和成熟,它与其它样品前处理技术的联用得到了迅速发展。与传统前处理方法相比,这些联用方法具有快速、高效、操作简便、节省溶剂、选择性好、应用范围广的特点。该文综述了微波辅助萃取及其与其它样品前处理技术联用的特点及适用性,并对近年来微波辅助萃取与其它前处理方法联用的发展概况及在分析领域中的应用情况进行了详细总结。     

《化学通报》网络版（Chemistry Online）2006年第6期论文摘要

[w061]微波辅助萃取装置的研究进展AdvancesontheSystemofMicrowave assistedExtraction汪军霞李攻科(中山大学化学与化学工程学院广州510275)微波辅助萃取作为一种高效省时的样品前处理技术,在分析化学领域有着广泛的应用。微波作为一种热源可以用不同方式辅助萃取过程,从而产     

微波辅助萃取应用研究进展

近年来关于微波辅助萃取(MAE)与其他各种样品前处理技术的结合使用,以及与多种检测技术在线联用的研究越来越多,此外离子液体等新型绿色溶剂作为萃取剂在MAE中的应用也开始得到广泛关注.本文综述了近几年微波辅助萃取在环境、天然产物提取、食品和药物分析领域的应用情况,并对其将来的发展进行了展望.     

样品前处理技术在气相色谱分析中的应用进展

气相色谱法是当前应用最广泛的分析技术之一。使用气相色谱对复杂基体进行分析时的样品前处理步骤往往繁琐耗时,易引起误差,已成为制约分析效率和准确度提升的关键环节。本文综述了2009-2013年几种主要的样品前处理技术,包括吹扫捕集、固相萃取、固相微萃取、液相微萃取技术以及微波辅助萃取、超声波辅助萃取等场辅助萃取技术在气相色谱分析中的应用研究进展。     

电场辅助样品前处理技术研究进展

样品前处理是样品分析过程的关键环节。目前各种微波、光、压力、超声波等场作用因能强化溶质传递、加速样品分离而被广泛地运用到样品前处理中。其中,电场辅助样品前处理技术能提高微痕量分析物萃取效率和选择性,已成为场辅助样品前处理技术的研究热点,并已在食品、环境、医药、生物等领域得到应用。该文综述了包括电场辅助膜萃取技术、电场辅助液相(微)萃取技术、电场辅助固相(微)萃取技术在内的电场辅助样品前处理技术的研究进展,并展望了其发展趋势。     

影响微波辅助萃取虎杖中白藜芦醇产率的一些重要操作参数

研究了溶剂类型以及萃取时间和温度、微波功率、虎杖颗粒大小和水分等主要操作参数对微波辅助萃取虎杖(po1ygonum cuspidatum)中白黎芦醇(Res)产率的影响。实验表明：由于甲醇和丙酮具有较高的介电常数和损耗因子，是微波辅助萃取Res的最佳选择。微波辅助萃取温度和时间以及虎杖颗粒大小的影响较显著，其次为虎杖样品水分。微波功率在所实验范围内(300-1200W)基本无影响。最佳的萃取条件为：温度80℃；时间15ｍin；微波功率800－900Ｗ；虎杖颗粒大小为0．45—0．30mm；水分含量约为20％。     

微波萃取技术

微波萃取技术在有机污染物和有害金属分离的研究和应用方面出现了令人鼓舞的进展。微波萃取方法具有方便、快速、试剂消耗低、回收率高和可用水作萃取溶剂的优点。本综述介绍了微波萃取技术的原理、方法、设备和应用研究现状。     

油料油脂酚类化合物测定中样品前处理技术的研究进展

该文主要综述了油料油脂酚类化合物测定中的样品前处理技术研究进展,包括液液萃取、超声波辅助萃取、微波辅助萃取、超临界流体萃取、固相萃取以及磁固相萃取等。比较了不同前处理技术的优缺点,并对油料油脂酚类化合物测定中样品前处理技术研究趋势进行了展望。     

ICP-MS法分析白花蛇舌草中16种无机元素初级形态

应用电感耦合等离子体质谱技术(ICP-MS),分析了白花蛇舌中16种无机元素的初级形态;并研究了微波辅助萃取、超声辅助萃取、恒温水浴萃取三种萃取方式对其溶出特性的影响。结果显示:白花蛇舌草中含有丰富的无机元素,这可能促进其有效成分作用的发挥。除Cu、Se外,其它元素的微波萃取的萃取效率最高;Mg、K、Ca、Mn、Ni、Se、Ba的溶解态含量较高,其他元素主要以悬浮态的形式存在于溶液中。     

微波辅助萃取与超声波萃取丹参中丹酚酸B的比较研究

本文对微波辅助萃取和超声波萃取丹参中丹酚酸B进行了比较研究,并用高效液相色谱法(HPLC)测定了丹参中丹酚酸B.考察了微波辅助萃取和超声波萃取参数的影响,在各自最佳萃取条件下进行了丹参中的丹酚酸B提取率的比对,结果表明:微波辅助萃取6 min的提取率高于超声波萃取30 min的提取率.微波辅助萃取法与超声波萃取法相比具有省时、高效和溶剂用量少的特点.利用指纹图谱比较了两种萃取方式提取的化学成分的差异,结果显示两种萃取方法提取的主要成分组成基本相同,其共有成分比例相近.     

Review of Analytical Methods for Atmospheric Oxidants Measurements

Abstract

Instrumental and manual methods currently available for the measurement of atmospheric oxidants are surveyed. Techniques used in the United States are emphasized and their advantages and disadvantages are discussed. Commercial systems are evaluated in terms of general operating principles rather than of specific instruments. The ability of these techniques to meet the measurement requirements defined by U.S. Federal air quality oxidant criteria are discussed. Alternative chemical techniques that may have some advantages over the neutral, buffered KI procedure are discussed. Also some attractive, alternative instrumental procedures that are ozone-specific are presented. These systems are based on chemiluminescence and ultraviolet absorption photometry. Electrochemical and colorimetric methods for total oxidant measurements are compared. Finally, some data are presented on relationships of ozone and total oxidants.     

Densities,speeds of sound,excess volumes and viscosities of binary mixtures of mtbe with tetralin and decalin at 303.15 k

Measurements of densities, speeds of sound, excess volumes and viscosities of binary mixture of methyl tert-butyl ether with tetralin and decalin are reported at 303.15?K over the entire range of composition. Excess volumes are measured using batch dilatometer technique. Sound speeds are obtained using ultrasonic interferometer. Densities are computed from excess volume data. Isentropic compressibilities are derived from density and sound speed data. Speeds of sound are evaluated on the basis of Jacobson's free length theory and Schaff's collision factor theory. The predicted values are in good agreement with the experimental results. The viscosity data are analysed on the basis of corresponding states approach. Excess volumes and deviation in isentropic compressibilities are negative and deviation in viscosities are positive over the entire composition range. The experimental results are discussed in terms of possible molecular interactions between unlike molecules.     

若干含多硫基的配合物的合成方法及结构特征

本文综述了近年来我们合成的十二种多硫基的配合物，这些配合物含有Ｓ＾２－２，Ｓ＾２－４，Ｓ＾２－５，Ｓ＾２－６，Ｓ＾２－７等多硫革配体，总结了这些配合物中的金属配位构型，比较了各种多硫基的Ｓ－Ｓ键长及有关键角，归纳了配合物外光谱，并阐述了其中几个配合物与ＮＨ２ＮＨ２的反应性能。     

钼、钨系过氧化物在Sharpless烯烃环氧化反应中的应用*

钼、钨系过氧化物是非常重要的Sharpless烯烃环氧化催化剂,有着非常广泛的工业发展前景。本文综述了钼、钨系过氧化物的种类,结构,合成方法及催化活性,分析了各种钼、钨系过氧化物的特点以及在催化环氧化领域的发展现状。同时,本文还讨论了钼、钨系过氧化物催化烯烃环氧化反应的机理。评述了在催化环氧化领域中两种主要理论——Mimoun机理与Sharpless机理的争论焦点及发展现状,以及计算化学对两种理论中间过渡态的研究进展,并且重点分析了Sharpless机理的过渡态结构。此外,本文还综述了影响钼、钨系过氧化物催化剂反应活性的各种因素以及质子所产生的副反应。最后,本文对应用于催化环氧化领域的钼、钨系过氧化物未来的研究方向提出了建议。     

Contactless conductivity detection for microfluidics: designs and applications

Different methods for construction of contactless conductivity detectors (CCD) for microchip electrophoresis device are described in this review. This includes three main schemes of CCD for microchips, such as (i) the detection electrodes are placed along the microchannel from outside of the microchip and they are insulated from the channel by the cover lid of microchip device; (ii) the electrodes are placed across of the microchannel in the same plane and they are insulated by thin separation channel walls and (iii) electrodes are buried in widened part of microchannel and they are insulated from solution by ultrathin layer of silicon carbide. Specific issues related to the CCD on microfluidics are discussed, such as an influence of shape and magnitude of ac voltage and placement of electrodes and their insulation. Various applications for security, pharmacological, bioassays and food analysis purposes are described.     

The Application of NMR Spectroscopy and Chemometrics in Authentication of Spices

Spices and herbs are among the most commonly adulterated food types. This is because spices are widely used to process food. Spices not only enhance the flavor and taste of food, but they are also sources of numerous bioactive compounds that are significantly beneficial for health. The healing effects of spices are connected with their antimicrobial, anti-inflammatory and carminative properties. However, regular consumption of adulterated spices may cause fatal damage to our system because adulterants in most cases are unhealthy. For that reason, the appropriate analytical methods are necessary for quality assurance and to ensure the authenticity of spices. Spectroscopic methods are gaining interest as they are fast, require little or no sample preparation, and provide rich structural information. This review provides an overview of the application of NMR spectroscopy combined with chemometric analysis to determine the quality and adulteration of spices.     

Some Strategies for the Refinement of Disordered Structures with the SHELXL-97 Refinement Program

1 INTRODUCTION finement stage. The person performing the crysta- llographic manipulations works on numerical data The high degree of order in the arrangement of that are quite different from the diffraction images atoms in a crystal is a fundamental characteristic of on a computer terminal, and most often does not even the crystalline state, an ideal crystal being envisaged see the images. to be constructed of regularly-stacked unit cells, each The refinement program, SHELXL-97[1], has …     

Alternate multi-layered adsorption of macro-cations and -anions on the colloidal spheres. Influence of the deionization of the complexation mixtures with coexistence of the ion-exchange resins

The alternate multiple adsorption layers of macrocations and macroanions on the surfaces of colloidal spheres, in which the complexation mixtures are deionized with ion-exchange resins are studied with help of the electrophoretic light-scattering, dynamic light-scattering and transmitted electron-microscopy techniques. The results are compared with those without resins. Colloidal silica spheres (110 nm in diameter) and monodispersed polystyrene spheres (220 nm) are used as colloidal spheres. The macrocations used are poly (4-vinyl-N-n-butyl pyridinium bromide) and poly (allylamine hydrochloride). Sodium poly (styrene sulfonate) and sodium polyacrylate are used as macroanions. The macroion-colloid complexations are formed firmly when the complexation suspensions are deionized with the resins.     

Indolizines and Their Hetero/Benzo Derivatives in Reactions of [8+2] Cycloaddition

Peculiarities of [8+2] cycloaddition of acetylenes to indolizines are reviewed. Especially mentioned are indolizines with leaving groups at positions 3 and 5. Cycloaddition to aza- and benzo derivatives are reviewed, as well as 1,10-cyclizations and processes leading to cyclazines where indolizines are intermediates. Mechanistic features (adducts and cycloadducts) and theoretical aspects (one- or two-steps mechanism) are reviewed.