Advances in sample preparation in chromatography for organic environmental pollutants analyses

Many pollutants are present at trace level in our environment, which are beyond the scope of the detection by advance instruments too. Therefore, there is urgent need to develop advance sample preparation methods to determine the concentrations of the pollutants even at trace levels. Keeping this into consideration, many extraction techniques have been developed and applied for the analysis of organic pollutants in environmental samples. This review presents the sate-of-the-art of sample preparation methods in environmental samples. The extraction techniques discussed are headspace, liquid based extraction, supported liquid, homogeneous liquid–liquid, homogeneous liquid–liquid, single drop micro-extraction, membrane assisted solvent, solid-phase, molecularly imprinted solid-phase, monolithic spin column, matrix solid-phase, dispersive solid-phase, disposable pipette, magnetic solid-phase, solid-phase micro-extraction, micro-extraction by packed sorbent and stir bar sorptive. The article will be highly useful for environmental chromatographers.     

糖肽的固相合成

目前糖肽的固相合成可以分为两种策略：构建单元策略和固相糖基化策略。本文对O-连接和N-连接糖肽固相合成的研究进展进行了综述。     

Tosylation of endocrine-disruptive alkylphenolic compounds in a solid-phase reaction system consisting of C18-modified silica gel and aqueous buffer solution

The tosylation reaction of endocrine-disruptive alkylphenolic compounds in a solid-phase aqueous system was investigated with the aim of developing an environment-friendly and efficient derivatization method for HPLC analyses of environmental samples. The phenols were rapidly and efficiently converted to the tosyl derivatives on a commercially available ODS solid-phase cartridge by passing an aqueous buffer solution through it. The solid-phase aqueous tosylation system has been incorporated into a preconcentration step performed by solid-phase extraction from environmental water.     

载体固相反应在多氮化合物合成中的应用

介绍了在载体固相反应中常用的固相载体以及多氮化合物的载体固相合成。参考文献10篇。     

Photochromic properties of phenanthroline-annulated spirooxazine in the solid state

Photochromic transformations of phenanthroline-annulated spirooxazine were observed in polycrystalline powders and solid-phase films obtained from solutions by solvent evaporation. The spectral and kinetic properties of the solid-phase films were studied by stationary absorption spectroscopy and laser flash photolysis. The mechanism of photoinitiated reactions of solid-phase samples of phenanthroline-annulated spirooxazine includes mutual transformations of different transoid isomers of the merocyanine form.     

Solid-Phase Synthesis of Nitrogen-Containing Five-Membered Heterocycles

In recent decades, a large number of reports related to solid-phase synthesis of heterocycles have appeared, owing to the wide variety of their biological activity. This review introduces the key concepts of solid-phase methodology and combinatorial synthesis with particular focus on the important role of solid-phase synthesis in the synthesis of nitrogen-containing five-membered ring heterocycles.     

拉曼光谱在固相有机合成中的应用

本文综述了近几年以来拉曼光谱在固相有机合成中的应用研究进展,分别介绍了近红外傅立叶变换和共焦显微两种拉曼光谱技术。近红外傅立叶变换拉曼光谱克服了荧光背景带来的干扰,可以用在固载试剂、催化剂的表征、固相有机反应的监测等方面,特别对于在无机载体上进行的有机反应的表征和检测方面具有很大的优势。共焦显微拉曼光谱具有特殊的空间分辨能力,适合对固相合成载体的结构进行表征,并可对载体内部反应活性位点的分布情况进行研究。     

衍生多孔碳材料在固相微萃取中的应用研究进展

固相微萃取是一种集采样、萃取、富集和进样于一体的样品前处理技术,其萃取效果与涂层材料密切相关。多孔碳材料具有比表面积大、多孔结构可控、活性位点多和化学稳定性好等优点,广泛应用于电池、超级电容器、催化、吸附和分离等领域,也是一种热门的用作固相微萃取探针的涂层材料。衍生多孔碳材料因种类丰富、可设计性强被广泛研究,研究主要集中在对衍生多孔碳材料的结构优化方面。但是衍生多孔碳材料在固相微萃取中的应用还存在如下问题:(1)共价有机框架衍生多孔碳材料的制备已取得较大进展,但将其应用于固相微萃取领域的研究仍较少;(2)有待进一步明确制备出的衍生多孔碳材料用作固相微萃取涂层表现出优异提取能力的机理;(3)有待进一步深入研究将衍生多孔碳材料用作固相微萃取涂层以实现对不同物理化学性质污染物的广谱高灵敏度分析。文章综述了近3年衍生多孔碳材料在固相微萃取中的应用研究,并展望了未来衍生多孔碳材料在固相微萃取中的研究前景。引用文献共56篇,主要来源于Elsevier。     

Enhanced sensitivity of LC-MS analysis of permethylated N-glycans through online purification

Aberrant glycosylation of proteins and lipids has been implicated in many human diseases, thus prompting the need for reliable analytical methods that permit dependable quantification of glycans originating from biological specimens. MS of permethylated glycans is currently employed to monitor disease-related aberrant glycosylation of proteins and lipids. However, enhancing the sensitivity of this type of analysis is still needed. Here, analysis of permethylated glycans at enhanced sensitivity is attained through miniaturized solid-phase permethylation and online solid-phase purification. Solid-phase permethylation method was miniaturized by reducing the amount of sodium hydroxide beads (one-third the original amount) packed in microspin columns. The efficiency of glycan permethylation was not adversely affected by this reduction. Online solid-phase purification of permethylated N-glycans derived from model glycoproteins, such as fetuin, α-1 acid glycoprotein and ribonuclease B, offered more sensitive and reproducible results than offline liquid-liquid and solid-phase extractions. Online solid-phase purification method described here permitted a 75% increase in signal intensities of permethylated glycans relative to offline purification methods. This is mainly due to the minimized sample handling associated with an online cleaning procedure. The efficiency and utility of online solid-phase purification was also demonstrated here for N-glycans derived from human blood serum. Online solid-phase purification permitted the detection of 73 N-glycan structures, while only 63 glycan structures were detected in the case of samples purified through liquid-liquid extraction. The intensities of the 63 structures that were detected in both cases were 75% higher for samples that were purified through the online method.     

Analysis of Volatile Compounds in Radix Bupleuri Injection by GC–MS–MS

Static headspace sampling, headspace solid-phase microextraction, and direct immersion solid-phase microextraction coupled with gas chromatography–tandem mass spectrometry have been developed for determination of the volatile components in Radix bupleuri injection. A total of 78 compounds were identified from Radix bupleuri injection. Direct immersion solid-phase microextraction gave a better extraction efficiency for polar compounds, including organic acids and alcohols, than headspace solid-phase microextraction or static headspace sampling. Product ion isotope pattern analysis was applied to determine the elemental composition of the precursor ion, which could make the qualitative analysis more accurate and reliable.     

The Comparison of Different Stationary Phases for the Analysis of Methamphtamine by Solid-phase Microextraction (SPME) and Gas Chromatography——Mass Spectrometry (GC/MS)

Methamphtamine is a kind of drug used as central nervous system stimulants, which has been widely abused. The drug is analyzed both for therapeutic value and in forensic medicine and toxicology. Though liquid-liquid extraction and solid-phase extraction are two kinds of common extractant method for the analysis of methamphtamine in urine,they both need high purity solvent. Recently, Lord et.al reported the method optimization for the analysis of amphetamines in urine by head-space solid-phase microextraction. Compareing with the liquid-liquid extraction and solid-phase extraction, solid-phase microextraction has the advantages of more simple, quick operation, high efficiency and solvent free.     

Qualitative and quantitative analyses of resin-bound organic compounds

Methods for qualitative and quantitative analyses of resin-bound organic compounds are essential tools for chemistry development in solid-phase combinatorial and parallel syntheses. Here we discuss the use of gel-phase 19F NMR, the fluoride ion-selective electrode method, and spectrophotometry for monitoring solid-phase reactions. Our results indicate that the application of these diverse methods for analyzing the outcome of solid-phase combinatorial synthesis are sensitive and conclusive.     

Parallel synthesis of 3-amino-4H-quinolizin-4-ones, fused 3-amino-4H-pyrimidin-4-ones, and fused 3-amino-2H-pyran-2-ones

On the basis of the enaminone methodology, libraries of 3-amino-4H-quinolizin-4-ones, fused 3-amino-4H-pyrimidin-4-ones, and fused 3-amino-2H-pyran-2-ones were synthesized by the solid-phase and by the solution-phase parallel synthesis. The solution-phase approach turned out to be advantageous over the solid-phase approach. The solution-phase synthesis afforded, in most cases, analytically pure products in high yields, whereas the solid-phase approach gave products in poor yields and in low purity.     

固相萃取技术在食品痕量残留和污染分析中的应用

食品痕量残留和污染分析中,样品的前处理极为重要,也是其难点所在。由于食品和农产品样品的多样性和复杂性,目前还没有一种前处理技术能够适合所有情况下的所有样品。本文对近年来发展起来的新型固相萃取技术如固相微萃取、搅拌棒吸附萃取、基质固相分散萃取、分子印迹固相萃取、免疫亲和固相萃取、整体柱固相萃取、碳纳米管固相萃取等在食品痕量残留和污染分析中的应用进行了综述,对未来的发展前景作了展望。     

Alternative solvents for elevated-temperature solid-phase parallel synthesis. Application to thionation of amides

A new class of higher-boiling solvents was investigated for elevated-temperature solid-phase parallel synthesis. Extremely low vapor pressures at high temperature and a broader range of solvent effect tuning make this new class of solvents an ideal choice for high-temperature parallel solid-phase synthesis. Benzyl benzoate is identified as a superior high-boiling solvent for parallel solid-phase Lawesson's thionation reactions.     

Microwave-assisted solid-phase synthesis of 2,5-diketopiperazines: solvent and resin dependence

Solid-phase synthesis of diketopiperazines (DKPs) was preformed using various combinations of resins (polystyrene, TentaGel, ArgoGel, and PEGA) and solvents (toluene, tert-butyl alcohol, water, and toluene/2-butanol (1:4, v/v). The DKPs were synthesized from solid-phase bound dipeptides via intramolecular aminolysis. Both thermal and microwave-assisted solid-phase synthesis of DKPs gave high yields of products independently of resin and organic solvent used; however, only the PEGA resin resulted in high yields of DKPs in water independent of heating method. The short reaction times, high yields, and the possibility to run reactions in water when an appropriate resin is used makes the microwave-assisted solid-phase synthesis the method of choice. The method should be suitable for solid-phase synthesis of diketopiperazine-based libraries.     

石墨烯应用于样品前处理的研究进展

样品前处理技术在样品分析中发挥着越来越重要的作用,而对分析物的富集能力和对样品基体的净化程度主要取决于高效的样品前处理材料,所以发展高性能的样品前处理材料一直是该领域的前沿研究方向。近年来,各类先进材料已经被引入样品前处理领域,发展了多种高性能的萃取材料。由于独特的物理化学性质,石墨烯已在各个研究领域获得广泛关注,在样品前处理领域也发挥着重要作用。基于高的比表面积、大的π电子结构、优异的吸附性能、丰富的官能团和易于化学改性等优点,石墨烯和氧化石墨烯基萃取材料被成功应用于各种样品的前处理,对不同领域中多种类型分析物表现出优异的萃取性能。该论文总结和讨论了近3年来石墨烯材料(石墨烯、氧化石墨烯及其功能化材料)在柱固相萃取、分散固相萃取、磁性固相萃取、搅拌棒萃取、纤维固相微萃取和管内固相微萃取等方面的研究进展。基于多种萃取机理如π-π、静电、疏水、亲水、氢键等相互作用,石墨烯萃取材料能够高效萃取和选择性富集不同类别的目标分析物,如重金属离子、多环芳烃、塑化剂、雌激素、药物分子、农药残留、兽药残留等。基于新型石墨烯萃取材料的各种样品前处理技术与多种检测技术如色谱、质谱、原子吸收光谱等联用,广泛应用于环境监测、食品安全和生化分析等领域。最后,总结了石墨烯在样品前处理领域中存在的问题,并展望了未来的发展趋势。     

Analyses of pesticides and their metabolites in foods and drinks

The importance of matrix pretreatment, sample extraction and clean-up in multiresidue methods for pesticide analyses is discussed, with emphasis on alternative new techniques attempted worldwide such as accelerated solvent extraction, microwave-assisted extraction, solid-phase extraction, solid-phase micro-extraction, matrix solid-phase dispersion, supercritical fluid chromatography, ultrasonic extraction and gel permeation chromatography. Detection employing capillary gas chromatography and high-performance liquid chromatography in conjunction with mass spectrometry, capillary electrophoresis, immunoassay techniques and others is summarized.