野生菌中鹅膏毒肽和鬼笔毒肽检验方法及样品处理技术研究进展

综述鹅膏毒肽和鬼笔毒肽检验方法及野生菌样品处理技术研究进展。食用蘑菇中毒事件多为误食鹅膏菌毒素所致，引起急性肝毒性中毒的致命蘑菇毒素主要为鹅膏毒肽和鬼笔毒肽。蘑菇毒素检测样品处理技术主要包括蛋白沉淀法、固相萃取技术、在线净化技术、免疫亲和技术等，检测方法主要包括快速检测法、毛细管电泳质谱联用法、高效液相色谱法、液相色谱质谱联用法等。快速检测法操作简便，适用于蘑菇毒素现场检测；毛细管电泳质谱联用法有高分辨率和高灵敏度的特点；高效液相色谱法在基层实验室广泛应用于蘑菇毒素的检测分析；液相色谱质谱联用法可准确的对蘑菇毒素进行定性和定量分析。通过比较这些技术和方法，可对实验室根据相对应的样本建立简单、快速、准确检测鹅膏毒肽的方法提供重要参考依据。     

干果类食品的样品前处理与分析检测方法研究进展

坚果、果脯等干果类食品含有丰富的营养成分,深受国内外广大消费者的喜爱。但这些食品在果实生产、加工、储运时会使用农药或产生霉变等,造成干果中农药、重金属、霉菌毒素或添加剂等有害成分残留,甚至超过国家限量要求,带来严重的食品安全问题。因此,加强干果类食品的质量监督具有重要的经济和社会意义。但干果类食品基质复杂,有害物质种类多,结构和性质差异大,含量低,其分析检测需要快速高效的样品前处理技术和准确灵敏的分析检测方法。该文主要综述了近十年来干果类食品中有害物质的样品前处理及分析检测方法研究进展。其中样品前处理方法主要包括各种场辅助萃取法、相分离法和衍生化萃取方法等。场辅助萃取法主要是借助超声波和微波场等外场(协同)作用加快干果中有害物质的溶出速度,提高其萃取效率。相分离法,包括固相(微)萃取、分散固相萃取和液相(微)萃取法等,具有溶剂消耗少、分离富集效率高的优势,是干果样品分析中较常使用的前处理方法。该文还重点介绍了干果中各类有害成分分析检测技术,主要包括色谱、原子光谱、无机质谱、电化学分析等常规实验室方法,以及一些适用于现场分析的快速检测技术,并以此为基础,展望了干果类食品中有害物质分析检测技术的发展趋势。     

泡腾辅助微萃取技术的开发与应用研究进展

泡腾辅助微萃取(EAM)技术是一种利用CO₂供体和H⁺供体反应产生CO₂气泡促进萃取剂快速分散、增大与目标物的接触面积，以实现高效萃取的新型样品预处理手段。该技术具有分散速率快、萃取效率高、使用成本低、应用范围广等优点。得益于萃取剂的快速发展，泡腾辅助微萃取方法的构建和应用范围研究日趋完善和多样，已广泛用于环境、食品、生物等样品的前处理领域。该前处理技术结合各类检测仪器构建新型快速的检测方法，成功实现了重金属离子、农药、内分泌干扰物、抗生素等污染物的检测。在EAM技术的构建中，常考查泡腾片剂的组成、溶液pH、萃取温度、萃取剂种类、萃取剂添加量、洗脱剂种类、洗脱剂体积、洗脱时间、循环使用次数等因素对方法的影响，重点依据线性范围、相关系数、富集因子、检出限、定量限等参数对方法进行评判，最后结合各类仪器检测方法，实现在实际样品检测中的应用。该文从EAM技术常用的萃取剂方面入手，综述了基于纳米材料、离子液体等新兴萃取剂的EAM方法的构建，以及与液相色谱、气相色谱、原子吸收光谱或质谱等大型仪器联用，用于复杂基质中有害物质检测的研究...     

国家“十五”科学仪器攻关重大项目子课题“全自动多路加温加压快速溶剂萃取仪（APSE）”通过验收

样品分析过程包括取样、样品制备与处理、分析测定、数据处理、总结报告等五个部分，通过统计发现样品处理所需时间占整个分析过程的61％，而分析测定的时间仅占6％。目前实验室所采用的样品前处理技术主要为传统的索氏提取、液．液萃取、微波萃取和超临界流体萃取等，这些技术耗时长，萃取效率低。发展高效快速的样品制备与自动化的前处理技术已成为现代分析化学研究的一个重要方向。     

典型卤代阻燃剂的样品处理技术及分析检测研究进展

卤代阻燃剂被广泛用作油漆、纺织品、电子器件的添加剂,由于其具有挥发性,能渗入并长久存在于环境中,在环境和食物链中积累,对人类和其他生物健康造成危害,现已被禁止或限制使用。因此,急需建立更加灵敏、准确的卤代阻燃剂残留分析方法。本文系统介绍了卤代阻燃剂的污染途径,以及近年来关于卤代阻燃剂残留样品前处理方法和检测技术,污染途径包括：土壤、水体、空气、灰尘和生物样品污染途径等;样品前处理方法包括：固相萃取、搅拌棒萃取、分子印迹萃取、磁性固相萃取、超临界流体萃取、加压液体萃取等;检测技术包括：气相色谱-质谱检测法、液相色谱-质谱检测法、免疫分析检测法、X射线荧光法等,并对卤代阻燃剂的分析检测技术进行了总结和展望。     

基于电驱动在线快速分离富集技术的研究进展

样品前处理能将待测物从复杂基质中预先分离富集出来,以提高分析方法的灵敏度、选择性和准确性,是复杂样品分析的关键步骤。样品前处理是一个非自发的、从无序到有序的熵减过程,不仅费时费力,还极易引起误差。向体系输入能量和降低体系熵值可以增强分离富集效果,加快样品制备过程。将电场引入在线样品前处理,既能向体系做功,又能驱动样品定向迁移,使前处理的熵减过程快速顺利进行,是快速样品制备的有效途径。基于电驱动的在线分离富集技术综合了多种加速策略：（1）以电场形式向体系输入能量,加速传质和传热过程;（2）采用电渗流、电泳等电驱动定向流实现样品在分离、富集、检测各步骤之间的定向迁移,保证样品前处理与检测顺利进行;（3）利用在线联用技术集成样品前处理与分析检测各步骤,从而提高自动化程度,减少人为误差;（4）通过微型化装置或微萃取方法提高样品制备效率,缩短样品制备时间。该文总结了近10年与基于电驱动的在线快速分离富集技术相关的90多篇文献,综述了该技术领域的研究进展,探讨了电驱动毛细管在线快速分离富集技术、电驱动芯片在线快速分离富集技术和电驱动膜萃取在线分离富集技术各自的优势和潜力,并展望了该类技术的发展与应用趋势。     

固体进样元素分析技术在农业领域的应用

重金属是农产品、农田土壤、肥料、饲料等农业样品中的重要污染物,传统的实验室分析方法需繁琐的前处理,耗时费力,无法满足重金属的快速检测需求。固体进样元素分析技术具有简化样品前处理、便捷、绿色、高效等优势,在农业领域中元素的快速检测分析中具有良好的应用前景。通过对固体进样元素分析技术,包括样品导入技术和电热蒸发、电感加热、激光烧蚀、X射线荧光光谱、激光诱导击穿光谱等固体进样分析系统进行综述,并对这些技术在农业领域中的应用做了进一步的梳理。固体进样分析技术已在农业样品中元素的快速检测、现场监测、风险评估等工作中发挥着举足轻重的作用,相信随着仪器研发、材料科学、机器学习等新兴技术的快速发展,其结构小巧、使用简单、分析迅速等优势将会充分发挥,为农业领域中质量安全监管提供一种更为有效、可靠的快速检测手段。     

固相微萃取技术与环境样品前处理

固相微萃取技术是80 年代末发展起来的一项新型的无溶剂化环境样品前处理技术, 它主要与气相色谱和高效液相色谱联用, 能快速和有效地分析环境样品中的痕量有机污染物。技术从出现至今主要在萃取装置(萃取纤维涂层)、萃取方式及后序分析仪器上有较大的发展和变化, 这使得技术的应用范围不断拓宽。通过对现有文献的总结, 本文还提出了固相微萃取技术今后的发展趋势。     

Research progress of the retrospective detection of organophosphorus nerve agent exposure using point-of-care testing techniqueEI北大核心CSCD

有机磷神经性毒剂(OPNA)是一类速杀性化学战剂,人员中毒后通过溯源检测来确定OPNA种类和剂量对于毒剂使用指证和人员救治非常重要。当前大部分溯源检测方法灵敏度高、特异性好,但因依赖大型设备限于实验室,不便于现场检测。随着现场快速检测(POCT)技术的发展和新识别分子的开发,大量OPNA中毒溯源现场检测技术被建立和应用。本文主要基于胆碱酯酶活性抑制、特异性识别和直接生化反应原理从3方面分析总结了OPNA中毒溯源POCT技术的研究进展和应用,展望了其未来发展趋势。     

新型样品前处理材料在环境污染物分析检测中的研究进展

针对复杂样品的分析和痕量目标物的检测,样品前处理是必不可少的,高效的样品前处理技术不仅可以去除或减小样品基质干扰而且能够实现分析物的富集,提高分析检测的准确性和灵敏度。近年来,固相萃取、磁分散固相萃取、枪头固相萃取、搅拌棒萃取、固相微萃取等高效的样品前处理技术已在环境污染物分析检测中获得广泛关注,萃取效率主要取决于萃取材料,所以新型的高效萃取材料一直是样品前处理研究领域的重要发展方向。该文总结和讨论了近年来新型样品前处理材料在环境污染物分析检测中的研究进展,主要聚焦在石墨烯、氧化石墨烯、碳纳米管、无机气凝胶、有机气凝胶、三嗪基功能材料、三嗪基聚合物、分子印迹聚合物、共价有机框架材料、金属有机框架材料以及它们的功能化萃取材料等。这些材料已经被应用于环境样品中不同类别污染物的萃取富集,如重金属离子、多环芳烃、塑化剂、烷烃、苯酚、氯酚、氯苯、多溴联苯醚、全氟磺酸、全氟羧酸、雌激素、药物残留、农药残留等。这些样品前处理材料具有高的表面积、大量的吸附位点,并涉及多种萃取机理如π-π、静电、疏水、亲水、氢键、卤键等相互作用。基于这些萃取材料的多种样品前处理技术与各类检测方法如色谱、质谱、原子吸收光谱、荧光光谱、离子迁移谱等相结合,已广泛应用于环境污染物的高灵敏分析检测。最后,该文总结了样品前处理发展中存在的问题,并展望了其未来在环境分析中的发展趋势。     

Methods of sample preparation for determination of pesticide residues in food matrices by chromatography–mass spectrometry-based techniques: a review

Much progress has been made in pesticide analysis over the past decade, during which time hyphenated techniques involving highly efficient separation and sensitive detection have become the techniques of choice. Among these, methods based on chromatographic separation with mass spectrometric detection have resulted in greater likelihood of identification and are acknowledged to be extremely useful and authoritative methods for determination of pesticide residues. Even with such powerful instrumental techniques, however, the risk of interference increases with the complexity of the matrix studied, so sample preparation before instrumental analysis is still mandatory in many applications, for example food analysis. This article summarizes the analytical characteristics of the different methods of sample-preparation for determination of pesticide residues in a variety of food matrices, and surveys their recent applications in combination with chromatographic mass spectrometric analysis. We discuss the advantages and the disadvantages of the different methods, address instrumental aspects, and summarize conclusions and perspectives for the future.     

Analytical methods for the determination of fluoroquinolones in solid environmental matrices

We present a critical review of the analytical procedures proposed in the past decade for the determination of fluoroquinolones (FQs) by chromatographic methods in solid environmental matrices. We emphasize the overall analytical procedure, from sampling to final detection. We devote special attention to sample preparation, highlighting the problems involved in the analysis of real complex matrices, mainly soil, sediment, manure and sludge. We compare the different extraction techniques in terms of efficiency, time taken and environmental impact, pointing out advantages and drawbacks. We provide an overview on the role of photochemistry in the degradation of FQs in soils and sediments, and we underline the central position of analytical chemistry in environmental monitoring because FQs are emerging pollutants.     

Novel analytical procedures for screening of drug residues in water, waste water, sediment and sludge

Traces of pharmaceuticals are continuously introduced into the aquatic environment mainly by sewage treatment plant effluents. Final data about their impact on the ecosystem are still partly missing. Progress in instrumental analytical chemistry has resulted in the availability of methods that allow a monitoring of these pollutants at ng L⁻¹ levels. In this review the state-of-the-art of residue analysis of pharmaceuticals by chromatographic and electrophoretic techniques is summarized. Improvements in detection limits over the past years have mainly been due to sophisticated mass spectrometric detection techniques. Furthermore, robust sample preparation and preconcentration protocols based on solid-phase extraction and related procedures have contributed significantly to the achievements observed so far. This review also covers several immunochemical approaches which may serve as an inexpensive alternative for quick screening of samples.     

A review of modern sample-preparation techniques for the extraction and analysis of medicinal plants

Sample preparation is the crucial first step in the analysis of herbs. In recent years there has been increasing interest worldwide in the use of alternative/herbal medicine for the prevention and treatment of various illnesses. Currently, however, quality-related problems (lack of consistency, safety, and efficacy) seem to be overshadowing the potential genuine health benefits of various herbal products. Thus, the development of "modern" sample-preparation techniques with significant advantages over conventional methods for the extraction and analysis of medicinal plants is likely to play an important role in the overall effort of ensuring and providing high-quality herbal products to consumers worldwide. In this article, recent developments and applications of modern sample-preparation techniques for the extraction, clean-up, and concentration of analytes from medicinal plants or herbal materials are reviewed. These modern techniques include solid-phase microextraction, supercritical-fluid extraction, pressurized-liquid extraction, microwave-assisted extraction, solid-phase extraction, and surfactant-mediated extraction.     

复杂色谱信号自动解析中的化学计量学方法

色谱及其联用技术日趋完善,并向自动化、高通量和快速的方向发展。化学计量学利用"数学分离"手段,可以实现色谱信号的自动化解析,已成为现代色谱分析中非常活跃的研究领域。但以往的化学计量学方法并不能完全有效地实现复杂色谱信号自动化解析。为此,自动化色谱解析算法成为科研工作者关心的重点,众多新型的自动化解析算法被提出。针对复杂一维色谱数据以及联用仪器得到的二维和更高维数据的自动化分析,化学计量学研究主要集中在自动色谱峰识别、背景以及基线漂移校正、色谱谱峰漂移校正以及重叠色谱峰的解析。该文对近十年来发展的复杂体系色谱信号自动化解析中化学计量学方法的原理与应用进行了总结与评述,比较了各类方法的优势与不足。在此基础上,针对当前色谱自动化分析过程中的难题对未来该领域的研究方向进行了展望。     

磁性复合材料在固相萃取食品中环境类雌激素的应用进展EI北大核心CSCD

环境类雌激素作为食品中一类典型的污染物,严重影响人体内分泌系统的功能与代谢。磁性固相萃取因其简洁高效、富集倍数高、适用范围广等优点,已被广泛应用于食品中环境类雌激素的富集检测。Fe_(3)O_(4)纳米粒子作为经典的磁固相萃取材料,易于形成大分子团聚物,影响其选择吸附性能,限制了磁固相萃取技术在食品中环境类雌激素的痕量分析。新兴的磁性复合材料可有效地解决上述问题,已成为磁固相萃取技术的研究热点之一。本文综述了近5年来新兴的磁性聚合物复合材料、磁性碳基复合材料和磁性金属-有机骨架复合材料在食品中环境类雌激素富集检测的应用进展。     

Catching the elusive persistent and mobile organic compounds: Novel sample preparation and advanced analytical techniques

Persistent and Mobile Organic Compounds (PMOCs) are emerging pollutants in the environment that have only been rarely detected in previous years due to the lack of analytical techniques available for their analysis. These compounds, being very polar, are able to spread through the surface waters, and reach groundwaters and drinking water sources. The challenges in the analysis of these compounds in water include their poor extraction efficiencies from environmental matrices and weak retention in conventional chromatographic columns. As a result, the toxicity and environmental fate of PMOCs are largely unknown. This review will examine recent developments in sorbent and chromatographic column technologies, and other sample preparation strategies that will enable analysis of PMOCs and advance our knowledge on their fate and transport in the environment. In addition, analysis of these compounds in water via liquid chromatography with tandem mass spectrometry (LC–MS/MS) are discussed in this review.     

Evaluation of the possibility of detecting benzenic pollutants by direct spectrophotometry on PDMS solid sorbent

Solid-phase extraction has become one of the most commonly used techniques for preconcentration of analytes from environmental samples. In the standard use of solid sorbent phases the extracted pollutants are subsequently eluted with a suitable organic solvent before chromatographic analysis. An alternative to this procedure is analysis of the adsorbed and concentrated pollutants by direct application of a spectroscopic method (fluorimetry or absorptiometry) to the phase. Although this method cannot be expected to give results as precise as those given by chromatographic methods, it might have valuable applications, particularly for "on site" pollution monitoring. This paper reports an evaluation of the capability of the method for the spectrophotometric detection of BTX (benzene, toluene, xylenes) in aqueous media and in contaminated atmospheres, with polydimethylsiloxane (PDMS) as sorbent. The tests performed, with the estimated detection limits, indicate that the method is relatively simple and easy to operate and sensitive enough for application to the monitoring of pollution both in water and in air in an industrial ambient atmosphere.