肉类食品中杂环胺检测的样品前处理及分析方法的研究进展

杂环胺是畜禽、鱼肉等食品在高温烹饪过程中生成的一类致癌、致突变化合物,高效、高选择性的样品前处理方法和高灵敏的分析方法是食品中痕量杂环胺分析检测的关键。本文综述了近年来溶剂萃取、固相萃取和固相微萃取等样品前处理方法,以及液相色谱、液相色谱-质谱等分析方法在食品中痕量杂环胺检测中的应用,结合现有研究对其发展趋势进行了展望。共引用文献51篇。     

食品中霉菌毒素样品前处理及分析方法研究进展

霉菌毒素广泛存在于食物和动物饲料中,可经食物链传递危及动物与人体健康,带来严重的食品安全问题。食品基体复杂,霉菌毒素结构多样、含量极低,其分离分析需要高效的前处理技术及快速灵敏的分析方法。该文综述了基于分子印迹聚合物、量子点材料、石墨烯类碳材料、生物材料等新型分离介质的固相(微)萃取、液相(微)萃取、免疫亲和层析、磁分离等样品前处理技术及液相色谱-质谱、免疫分析法、生物传感器等分析方法在食品霉菌毒素分析中的应用,并展望了其发展趋势。     

体液的在线样品前处理技术及其小分子化合物的液相色谱-质谱分析

在线样品前处理液相色谱-质谱联用技术为体液中痕量小分子化合物提供了高灵敏度、高选择性和高通量的分析方法。该文以在线固相萃取柱为主线,总结了不同种类富集柱的特点及其近5年来在相关领域的应用,并简要介绍了在线液相色谱-质谱分析的流路系统。     

食品中真菌毒素样品前处理方法的研究进展

真菌毒素是由真菌在一定环境条件下产生的一类具有毒性的小分子次级代谢产物。真菌毒素种类多,毒性强,污染范围广,可经食物链直接或间接进入人体,危及人体健康。食品基质形态多样,成分复杂,而实际样品中真菌毒素含量低,难以直接对目标物进行分析,故高效的样品前处理技术能实现待测物的分离和富集,在实际样品的分析中尤为重要。该文主要综述了基于磁性纳米材料、石墨烯类材料、分子印迹材料、免疫亲和材料、适配体功能材料等新型分离介质的液相萃取技术、固相萃取技术、场辅助提取技术（磁性固相萃取、超声辅助提取、微波辅助提取）、免疫亲和柱法、QuEChERS法等前处理技术在食品中真菌毒素分析中的应用,并对其分析的发展趋势进行了展望。     

功能化有序介孔二氧化硅材料在分析样品前处理中的应用

功能化有序介孔二氧化硅材料具有均一可调的介孔孔径、规则的孔道、稳定的骨架结构、易于修饰的内表面和较高的比表面积、高的吸附容量等特性,可用于生物、医药、环境样品等复杂基体中痕量分析物的高选择性分离与富集,因此在样品前处理中的应用特别引人瞩目。文中简要介绍了功能化有序介孔二氧化硅材料的制备方法,综述了功能化有序介孔二氧化硅材料在分离富集金属离子、有机污染物以及生物大分子样品前处理中的应用进展。     

环境水样及固相样品中全氟化合物分析方法研究进展

全氟化合物(Perfluorinated compounds,PFCs)是一类持久性有机污染物,在环境中普遍检出,严重危害人体健康,已成为环境科学和毒理学研究的热点之一.PFCs含有较多同系物及同分异构体,且在环境中通常为痕量水平(ng/g或μg/L),迫切需要建立灵敏可靠的样品前处理和检测技术.国内外已针对环境样品基质中痕量PFCs的检测开展了大量研究,但有关复杂环境样品中PFCs前处理方法、分析方法、基质效应等方面的系统评述还相对较少.本文综述了环境样品(水、沉积物/污泥、土壤、植物)中PFCs的前处理方法、检测方法(尤其是同分异构体)及环境样品基质效应对其检测的影响,以期为相关研究提供参考.     

生物相容性分离介质在样品前处理中的应用

生物样品基体复杂,蛋白质等生物大分子的干扰给样品前处理带来很大的困难.近年来,生物相容性分离介质在样品前处理中的应用特别引人注目.本文综述了生物相容性分离介质及其在固相萃取、固相微萃取、微透析样品前处理中应用的进展.     

样品前处理介质的制备与应用研究进展

样品分析是环境污染物研究和控制的基础,到目前为止,环境样品前处理仍是环境样品分析的瓶颈问题,其中,针对复杂环境基质中的痕量污染物开发高效率和高选择性的吸附材料是样品前处理的关键和研究热点。微孔有机聚合物、有序介孔硅材料、金属有机骨架聚合物、分子印迹聚合物、碳纳米管和石墨烯等新材料具有骨架密度低、比表面积大、孔尺寸可调控、表面可修饰、化学和物理性质稳定等优点,在样品前处理领域展现出巨大的应用潜力。该文对近年来这些新型纳米材料在固相萃取、分散固相萃取、固相微萃取、磁固相萃取、搅拌棒吸附萃取和基质固相分散萃取等样品前处理领域的最新研究进展做了简要评述,为更好地开发新型纳米材料在复杂和痕量样品前处理中的应用提供了参考。     

分子印迹技术在样品前处理中的应用

分子印迹聚合物具有选择性高、稳定性好及制备简单的特点,可用于生物、医药、环境样品等复杂基体中痕量分析物的高选择性分离与富集,因此在样品前处理中的应用特别引人关注.本文介绍了分子印迹技术的基本原理,综述了分子印迹技术在样品前处理中应用的研究进展.     

磁性微纳米材料的功能化及其在食物样品前处理中的应用进展

磁性固相萃取是当前对复杂样品中痕量目标物进行有效分离富集的热门技术,功能化磁性微纳米粒子是该技术应用中的关键材料。本文综述了各种已报道的功能化磁性微纳米材料,总结了包括表面嫁接有机小分子、表面包覆碳或无机氧化物、表面嫁接或包覆聚合物、载体表面或孔道内负载磁性纳米粒子、载体骨架内掺入磁性纳米粒子、物理共混法制备磁性功能材料在内的6种功能化方法,并对功能化磁性微纳米材料在食物样品前处理中的应用进行了简要评述。     

Development and application of a high-performance liquid chromatography-mass spectrometry method to determine alendronate in human urine

Despite the high potential offered by electrospray ionization on highly polar compounds like biphosphonates, few applications have been developed. High-performance liquid chromatography (HPLC) separation methods suitable for such molecules cannot be used in tandem with mass spectrometry (MS) due to high non-volatile salt content; at the same time the sample preparation, in biological fluids, is also a challenging problem. In the past ion-pair chromatography was mainly used in the case of HPLC-MS of biphosphonates, but no application to quantitative pharmacokinetic (PK) studies has been presented. In this study, after preliminary tests with ion-pair chromatography showing a poor sensitivity, a combined derivatization of the amino group and the biphosphonate has been developed and tested in a PK study. Using this analytical approach we were able to fully validate the quantitation of alendronate in the range of 6.667-4860.0 ng/ml in urine (sample volume 2.0 ml); each analytical run was 5.0 min long. The sensitivity achieved permitted a correct evaluation of the alendronate urinary excretion over the full period of urine collection. Sample preparation despite its complexity permitted to process and analyze up to 200 samples in a working day.     

Quaternary ammonium pesticides: A review of chromatography and non-chromatography methods for determination of pesticide residues in water samples

The monitoring of pesticide residues in water sources is essential because of their increased worldwide demand in agriculture and their subsequent detection in waters. Pesticide residues in water matrices are traditionally determined by multiresidue methodologies based on chromatography coupled to mass spectrometry. However, for quaternary ammonium pesticide residues, as highly polar compounds, the chromatographic approach frequently fails, requiring modifications in the separation method, or even an alternative technique for analyte quantification. Therefore, to solve this analytical limitation for these residues, several authors proposed unusual methodologies, such as those based on spectroscopic or electroanalytical approaches. This review intends to offer an overview of the analysis of quaternary ammonium pesticide residues in different water sources, focusing on advances in sample preparation before chromatographic separations and alternative analytical techniques, such as spectroscopy and electroanalytical methods.     

Turbulent flow chromatography in bioanalysis: a review

With advances in fast chromatography techniques, and highly sensitive and selective detection methods such as tandem mass spectrometry, very high-throughput bioanalytical methods can now be easily developed. The bottleneck of the analytical process then becomes the sample preparation, which it is now realized is crucial to the robust operation of the analytical system, especially for quantitative assays. Turbulent flow liquid chromatography was developed in the late 1990s, and combines 'size exclusion' and traditional stationary phase column chemistry to separate macromolecules, such as proteins, from smaller molecules and analytes of interest in biological fluids. By definition, the process is very rapid, and the instrumentation and software have been developed for fully automated, on-line extraction of neat biological fluids. This work aims to review the chromatographic theory of turbulent flow chromatography and illustrate, using examples from recent literature, the application of this technique to a range of analytes from a number of different biological matrices.     

Miniaturized sample preparation combined with liquid phase separations

Miniaturized sample preparation methods designed as the sample pretreatment for liquid phase separations, such as liquid chromatography, capillary electrophoresis and capillary electrochromatography, have been reviewed especially for the on-line coupling of the sample preparation process and the separation process. The development of the desorption interfaces for the effective combining of the sample preparation and subsequent liquid phase separations is briefly described along with the applications of the combined analytical systems to the analysis of complex sample mixtures such as biological and environmental matrices. Novel use of fine polymeric filaments as the extraction medium for microscale liquid phase separation methods are investigated and a comparison is made with other sample preparation techniques. Polymer coating onto the fibrous material is also introduced to further develop microscale sample preparation methods with improved extraction performance. Several other microscale sample preparation methods having a potential compatibility to the liquid phase separations are also described for future applications of these techniques.     

Modern automated microextraction procedures for bioanalytical,environmental, and food analyses

Sample preparation frequently is considered the most critical stage of the analytical workflow. It affects the analytical throughput and costs; moreover, it is the primary source of error and possible sample contamination. To increase efficiency, productivity, and reliability, while minimizing costs and environmental impacts, miniaturization and automation of sample preparation are necessary. Nowadays, several types of liquid-phase and solid-phase microextractions are available, as well as different automatization strategies. Thus, this review summarizes recent developments in automated microextractions coupled with liquid chromatography, from 2016 to 2022. Therefore, outstanding technologies and their main outcomes, as well as miniaturization and automation of sample preparation, are critically analyzed. Focus is given to main microextraction automation strategies, such as flow techniques, robotic systems, and column-switching approaches, reviewing their applications to the determination of small organic molecules in biological, environmental, and food/beverage samples.     

Applications of Poly(Ethylene)Glycol (PEG) in Separation Science

The wide range of applications of poly(ethylene)glycol (PEG) in primarily chromatography and other closely related analytical methods has been reviewed. PEG has been used as mobile phase modifier in capillary electrophoresis (CE) as well as ion exchange, size exclusion, and hydrophobic interaction liquid chromatography (LC) methods. Generally in the presence of PEG, LC retention of macromolecules is altered and stability of their structure is maintained. PEG was effective in CE as a permanent coating for fused silica capillaries to shield free silanol groups that can cause protein adsorption to the wall resulting in band broadening and low recovery of the separated proteins. In gas chromatography, PEG-based stationary phases were applied for separation of polar analytes. PEG could also serve as an extraction medium in solid phase microextraction and aqueous two phase systems. Selected analytical applications, primarily LC and CE, involving PEG to facilitate the determination of either small molecules or macromolecules such as proteins in their native form are discussed and representative figures provided.

     

Extraction techniques based on solid state and connected with liquid chromatography

Extraction methods applied in analysis of water samples can be named as liquid chromatography. Very often, these techniques are used as sample preparation method before another analytical method such gas chromatography or high performance liquid chromatography. The subject of this review is to compare the extraction techniques of liquid samples and discuss their characteristics in comparison with liquid chromatography. Some new extraction techniques are described, and some characteristic parameters are compared.     

Analysis of bile acids in human biological samples by microcolumn separation techniques: A review

Bile acids are a group of compounds essential for lipid digestion and absorption with a steroid skeleton and a carboxylate side chain usually conjugated to glycine or taurine. Bile acids are regulatory molecules for a number of metabolic processes and can be used as biomarkers of various disorders. Since the middle of the twentieth century, the detection of bile acids has evolved from simple qualitative analysis to accurate quantification in complicated mixtures. Advanced methods are required to characterize and quantify individual bile acids in these mixtures. This article overviews the literature from the last two decades (2000–2020) and focuses on bile acid analysis in various human biological samples. The methods for sample preparation, including the sample treatment of conventional (blood plasma, blood serum, and urine) and unconventional samples (bile, saliva, duodenal/gastric juice, feces, etc.) are shortly discussed. Eventually, the focus is on novel analytical approaches and methods for each particular biological sample, providing an overview of the microcolumn separation techniques, such as high-performance liquid chromatography, gas chromatography, and capillary electrophoresis, used in their analysis. This is followed by a discussion on selected clinical applications.     

HPLC测定煤焦油中极性化合物的研究

应用高效液相色谱以正相－ＨＰＬＣ配以反冲（ＢＦ）技术,测定了煤焦油中极性化合物的总量。以反相（ＲＦ）－ＨＰＬＣ辅以制备液体色谱研究了极性段份的制备及典型极性化合物的分析,文中分析的实样由山西省一些焦化厂提供。     

Recent advances in metal‐organic frameworks and covalent organic frameworks for sample preparation and chromatographic analysis

In the field of analytical chemistry, sample preparation and chromatographic separation are two core procedures. The means by which to improve the sensitivity, selectivity and detection limit of a method have become a topic of great interest. Recently, porous organic frameworks, such as metal‐organic frameworks (MOFs) and covalent organic frameworks (COFs), have been widely used in this research area because of their special features, and different methods have been developed. This review summarizes the applications of MOFs and COFs in sample preparation and chromatographic stationary phases. The MOF‐ or COF‐based solid‐phase extraction (SPE), solid‐phase microextraction (SPME), gas chromatography (GC), high‐performance liquid chromatography (HPLC) and capillary electrochromatography (CEC) methods are described. The excellent properties of MOFs and COFs have resulted in intense interest in exploring their performance and mechanisms for sample preparation and chromatographic separation.