Analytical methods

分析方法
  • 文章类型: Journal Article
    水凝胶由三维(3D)和复杂的聚合物网络组成,这些网络决定了它们的物理性质。在水凝胶的结构分析方法中,在纳米尺度上对水凝胶的聚合物网络进行真实空间成像是最佳方法之一;然而,这是非常具有挑战性的。在这项研究中,我们提出了一种使用透射电子显微镜(TEM)直接观察阳离子聚合物网络的方法。通过结合双网络策略和矿物染色技术,我们克服了聚合物聚集和聚合物电子密度低的挑战。将目标阳离子网络掺入中性骨架网络中以抑制随后染色期间的收缩。沿着阳离子聚合物链的二氧化钛矿化为用于TEM观察的目标聚合物网络提供了足够的电子密度。这种观察方法可以实现真实空间中局部结构的可视化,并与散射方法在软物质结构分析中起到补充作用。
    Hydrogels consist of three-dimensional (3D) and complicated polymer networks that determine their physical properties. Among the methods for structural analyses of hydrogels, the real-space imaging of a polymer network of hydrogels on a nanometer scale is one of the optimal methods; however, it is highly challenging. In this study, we propose a direct observation method for cationic polymer networks using transmission electron microscopy (TEM). By combining the double network strategy and the mineral staining technique, we overcame the challenges of polymer aggregation and the low electron density of the polymer. An objective cationic network was incorporated into a neutral skeleton network to suppress shrinkage during subsequent staining. Titania mineralization along the cationic polymer strands provided sufficient electron density for the objective polymer network for TEM observation. This observation method enables the visualization of local structures in real space and plays a complementary role to scattering methods for soft matter structure analysis.
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  • 文章类型: Journal Article
    液晶单体(LCM)是一类新兴的污染物,预计具有持久性,生物蓄积性和毒性(PBT)。作为液晶显示器(LCD)的关键部件之一,含有LCD的器件的处理与LCM向环境中的排放密切相关。LCM已经在包括灰尘在内的各种环境基质中被检测到,沉积物,土壤,污水渗滤液,和空气,室内住宅粉尘中的浓度范围在17至2121纳克/克之间。此外,在人体皮肤和电子废物拆解工人血清中检测到的浓度高达2,071,000纳克/平方米,浓度范围为3.9至276ng/mL。尽管这些化合物受到了深远的污染,他们对环境行为的了解有限,命运,和毒性。模型预测表明,330个LCM中有297个是持久性和生物蓄积性化合物,还有更多的被认为是有毒的。然而,目前对其物理化学和PBT性质的了解在很大程度上仅限于理论预测,并且仅限于少量的实验毒性研究。作为一种新兴的污染物,研究之间缺乏标准化被认为是提高这些化合物知识水平的关键挑战.不仅在环境介质中确定和量化的统一分析方法尚未建立,但也需要一个通用的缩写系统。为了进一步协调LCM的数据报告,我们建议报告十个优先LCM的总集中,根据检测频率选择,毒性和人体暴露的潜力。在十个优先LCM中,有五个是氟化联苯和类似物,四个是联苯/双环己基和类似物,一个是氰基联苯。
    Liquid crystal monomers (LCMs) are a class of emerging contaminants of concern predicted to be persistent, bioaccumulative and toxic (PBT). Being one of the key components in liquid crystal displays (LCDs), the disposal of LCD containing devices is closely related to the emission of LCMs into the environment. LCMs have been detected in a wide range of environmental matrices including dust, sediment, soil, sewage leachate, and air, with concentration ranges between 17 and 2121 ng/g found in indoor residential dust. Furthermore, they have been detected on human skin at concentrations up to 2,071,000 ng/m2 and in the serum of e-waste dismantling workers, at concentrations ranging from 3.9 to 276 ng/mL. Despite the far-reaching contamination of these compounds, there is limited knowledge of their environmental behaviour, fate, and toxicity. Model predictions show that 297 of 330 LCMs are persistent and bioaccumulative compounds, with many more indicated as being toxic. However, current knowledge of their physicochemical and PBT properties is largely restricted to theoretical predictions and limited to a small number of experimental toxicity studies. As an emerging class of contaminants of concern, a lack of standardisation between studies was identified as a key challenge to advancing the state of knowledge of these compounds. Not only are harmonised analytical methods for their determination and quantification in environmental media yet to be established, but there is also a need for a universal abbreviation system. To further harmonise the reporting of data on LCMs we propose reporting the sum concentration of ten priority LCMs, selected on the basis detection frequency, toxicity and potential for human exposure. Of the ten priority LCMs five are fluorinated biphenyls and analogues, four are biphenyls/bicyclohexyls and analogues and one is a cyanobiphenyl.
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  • 文章类型: Journal Article
    分子齿轮系统是宏观世界中复杂齿轮机械的技术模拟纳米级类似物,同样被定义为包含通过机械接合执行相关旋转运动的相互啮合元素的系统。只是最近,已经开发了主动驱动分子齿轮运动而不是依靠被动热激活的新方法。这项工作的进一步进展将为单向分子齿轮装置铺平道路,该装置具有等待实现的独特类型的分子机器。在这项工作中,通过证明分子光凝胶系统1中光诱导旋转的方向偏差,实现了实现这一目标的重要步骤。使用定制设计的LED耦合手性低温HPLC设置对映体分析物的原位辐照,通过实验阐明了顺时针或逆时针旋转的固有选择性。对于光凝胶1,观察到光凝胶过程和光诱导的单键旋转(SBR)中的显着方向偏差,方向偏好高达4.8:1。利用这些效应将允许在未来合理地设计和构造完全定向的分子齿轮传动马达。
    Molecular gearing systems are technomimetic nanoscale analogues to complex geared machinery in the macroscopic world and are likewise defined as systems incorporating intermeshed elements which perform correlated rotational motions by mechanical engagement. Only recently, new methods to actively drive molecular gearing motions instead of relying on passive thermal activation have been developed. Further progress in this endeavor will pave the way for unidirectional molecular gearing devices with a distinct type of molecular machine awaiting its realization. Within this work an essential step towards this goal is achieved by evidencing directional biases for the light-induced rotations in molecular photogear system 1. Using a custom-designed LED-coupled chiral cryo-HPLC setup for the in-situ irradiation of enantiomeric analytes, an intrinsic selectivity for clockwise or counterclockwise rotations was elucidated experimentally. Significant directional biases in the photogearing processes and light-induced single bond rotations (SBRs) are observed for photogear 1 with directional preferences of up to 4.8:1. Harnessing these effects will allow to rationally design and construct a fully directional molecular gearing motor in the future.
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  • 文章类型: Journal Article
    硝基酚,一个多才多艺的中间体,已广泛用于皮革,医学,化学合成,和其他领域。因为这些部件应用广泛,他们可以通过各种途径进入环境,导致许多危害和毒性。最近简单的发展激增,快速,环保,以及确定这些环境污染物的有效技术。本文综述了2017年以来硝基苯酚的前处理和分析方法的最新研究进展,并以环境样品为重点。预处理方法包括液-液萃取,固相萃取,分散提取,和微萃取方法。分析方法主要包括液相色谱法,基于气相色谱的方法,超临界流体色谱.此外,本文还讨论和比较了不同预处理和分析方法的优缺点和发展前景,为进一步研究提供参考。
    Nitrophenols, a versatile intermediate, have been widely used in leather, medicine, chemical synthesis, and other fields. Because these components are widely applied, they can enter the environment through various routes, leading to many hazards and toxicities. There has been a recent surge in the development of simple, rapid, environmentally friendly, and effective techniques for determining these environmental pollutants. This review provides a comprehensive overview of the latest research progress on the pretreatment and analysis methods of nitrophenols since 2017, with a focus on environmental samples. Pretreatment methods include liquid-liquid extraction, solid-phase extraction, dispersive extraction, and microextraction methods. Analysis methods mainly include liquid chromatography-based methods, gas chromatography-based methods, supercritical fluid chromatography. In addition, this review also discusses and compares the advantages/disadvantages and development prospects of different pretreatment and analysis methods to provide a reference for further research.
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  • 文章类型: Journal Article
    微塑料(MPs)和金属由于其持久性和对生态系统和人类健康的潜在威胁,目前是最值得关注的两种环境污染物。这篇综述研究了不同环境隔室中MP和金属之间的复杂相互作用,包括水生,陆地,通过关注吸附和解吸的复杂过程以及控制这些相互作用的机制,以及大气环境。国会议员在水生和陆地环境中充当金属的载体和集中器,影响这些污染物对水生和陆生生物的生物利用度和毒性。这篇综述强调了与当前分析方法相关的现有挑战和制约因素,包括显微镜,光谱学,和等温线模型在研究微塑料-重金属相互作用中的应用。此外,我们确定了知识差距和未来的研究方向,可以增强我们对各种环境环境中MP和金属之间的动态相互作用的理解。
    Microplastics (MPs) and metals are currently two of the most concerning environmental pollutants due to their persistent nature and potential threats to ecosystems and human health. This review examines the intricate interactions between MPs and metals in diverse environmental compartments, including aquatic, terrestrial, and atmospheric environments by focusing on the complex processes of adsorption and desorption and the mechanisms that govern these interactions. MPs act as carriers and concentrators of metals in aquatic and terrestrial environments, affecting the bioavailability and toxicity of these contaminants to aquatic and terrestrial organisms. This review highlights the existing challenges and constraints associated with current analytical methods, including microscopy, spectroscopy, and isotherm models in studying microplastic-heavy metal interactions. Moreover, we identified the knowledge gaps and future research directions that can enhance our understanding of the dynamic interplay between MPs and metals in various environmental settings.
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  • 文章类型: Journal Article
    挥发性组学是一个科学领域,涉及评估食品基质中的挥发性化合物及其鉴定方法。这篇综述讨论了塑造葡萄酒香气的主要化合物组,他们的起源,前体,和选定的代谢途径。本文将水果酒分为几类,包括苹果酒和苹果酒,樱桃葡萄酒,李子酒,浆果葡萄酒,柑橘葡萄酒,和异国情调的葡萄酒。以下文章讨论了塑造每组葡萄酒香气的挥发物的特征以及它们出现的浓度。它还讨论了酵母和乳酸菌的菌株和种类如何影响果酒的香气。本文还涵盖了评估水果葡萄酒挥发性化合物分布的技术,包括现代分析技术。
    Volatilomics is a scientific field concerned with the evaluation of volatile compounds in the food matrix and methods for their identification. This review discusses the main groups of compounds that shape the aroma of wines, their origin, precursors, and selected metabolic pathways. The paper classifies fruit wines into several categories, including ciders and apple wines, cherry wines, plum wines, berry wines, citrus wines, and exotic wines. The following article discusses the characteristics of volatiles that shape the aroma of each group of wine and the concentrations at which they occur. It also discusses how the strain and species of yeast and lactic acid bacteria can influence the aroma of fruit wines. The article also covers techniques for evaluating the volatile compound profile of fruit wines, including modern analytical techniques.
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  • 文章类型: Journal Article
    水体在支持生命中起着至关重要的作用,维护环境,保护印度人民的生态。然而,近几十年来,人类活动导致了水生环境的各种变化,通过污染导致环境恶化。由于人口的快速增长和工业的扩张,将地表水源用于饮用和其他目的的安全性受到了严格的审查。微塑料(MPs)(塑料尺寸<5毫米)引起的地表水污染是发展中国家大都市中新兴的污染物之一,因为它具有最大的弹性和合成性质。最近对地表水体的研究(河流,池塘,湖等。)描绘了MP水平与不同污染参数(如电导率)之间的相关性,总磷酸盐,和生物需氧量。纤维代表在地表水体中发现的MP的主要形式,表现出不同季节的波动。因此,本研究优先考虑理解适应,患病率,属性,波动,以及沉积物和地表水环境中MPs的空间分散。此外,该研究旨在确定当前理解中存在的差距,并强调未来调查的机会。从目前的研究来看,据报道,南中国海西沙群岛的MP浓度在0.2-45.2项目/升范围内,而在印度,在水样中发现了96个项目/L,在沉积物样品中发现了259个项目/kg。这无疑将有助于城市规划者实现可持续发展目标,以减轻不断增加的新兴污染物负荷。
    Water bodies play a crucial role in supporting life, maintaining the environment, and preserving the ecology for the people of India. However, in recent decades, human activities have led to various alterations in aquatic environments, resulting in environmental degradation through pollution. The safety of utilizing surface water sources for drinking and other purposes has come under intense scrutiny due to rapid population growth and industrial expansion. Surface water pollution due to micro-plastics (MPs) (plastics < 5 mm in size) is one of the emerging pollutants in metropolitan cities of developing countries because of its utmost resilience and synthetic nature. Recent studies on the surface water bodies (river, pond, Lake etc.) portrait the correlation between the MPs level with different parameters of pollution such as specific conductivity, total phosphate, and biological oxygen demand. Fibers represent the predominant form of MPs discovered in surface water bodies, exhibiting fluctuations across seasons. Consequently, present study prioritizes understanding the adaptation, prevalence, attributes, fluctuations, and spatial dispersion of MPs in both sediment and surface water environments. Furthermore, the study aims to identify existing gaps in the current understanding and underscore opportunities for future investigation. From the present study, it has been reported that, the concentration of MPs in the range of 0.2-45.2 items/L at the Xisha Islands in the south China sea, whereas in India it was found in the range of 96 items/L in water samples and 259 items/kg in sediment samples. This would certainly assist the urban planners in achieving sustainable development goals to mitigate the increasing amount of emergent pollutant load.
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  • 文章类型: Journal Article
    预期纳米塑料在各种环境隔室中普遍存在。然而,分析方法的挑战阻碍了我们对与特定纳米塑料特性(如尺寸和化学成分)相关的风险的理解,以及纳米塑料和微生物之间的相互作用。在这项研究中,我们应用适合目的的分析方法和技术来了解纳米塑料化学成分如何影响它们与从活性污泥中收集的细菌的相互作用。当暴露于聚苯乙烯(PS)和聚氯乙烯(PVC)纳米塑料5天时,纳米塑料附着在细菌上。具体来说,在第1天,PS纳米塑料明显优于尺寸和形状相似的PVC,可能是由于化学成分的差异。5天后,附着在细菌上的纳米塑料大幅减少,提示细菌防御机制可能会随着时间的推移减少颗粒附着。总体细菌群落结构表现出高度的恢复力。这种复原力突出了微生物群落维持其结构的能力,尽管有纳米塑料压力,一致的阿尔法多样性证明了这一点,PCoA,和PERMANOVA结果。了解这些机制对于评估纳米塑料的命运和环境影响至关重要。
    Nanoplastics are anticipated to be ubiquitous in various environmental compartments. However, challenges in analytical methods hinder our understanding of risks related to specific nanplastics characteristics such as size and chemical compositions, and interactions between nanoplastics and microorganisms. In this study, we applied fit-for-purpose analytical methods and techniques to understand how nanoplastic chemical composition influences their interaction with bacteria collected from activated sludge. When exposed to polystyrene (PS) and polyvinyl chloride (PVC) nanoplastics for 5 days, the nanoplastics attached to the bacteria. Specifically, on day 1, there was a significant predominance of PS nanoplastics over PVC ones of similar size and shape, possibly due to differences in their chemical composition. After 5 days, there is a substantial decrease in nanoplastics attached to bacteria, suggesting bacterial defence mechanisms may reduce particles attachment over time. The overall bacterial community structure demonstrated a high degree of resilience. This resilience highlights the ability of microbial communities to maintain their structure despite nanoplastic stressors, as evidenced by consistent alpha diversity, PCoA, and PERMANOVA results. Understanding these mechanisms is crucial for assessing nanoplastic fate and thus environmental impacts.
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  • 文章类型: Journal Article
    欧盟最近决定将草甘膦的使用授权延长至2033年12月15日,这激发了全世界关于其毒性或其他对人类的科学讨论。草甘膦是一种化学物质,在过去的50年中,全球已使用数百万吨来干燥耕地和温室以及路边的杂草。在许多领域,人们对它可能在食物链中的存在及其对健康的不利影响表示关注。在这里讨论了支持毒性的两个方面,以及那些可能表明草甘膦毒性有限的方面。已经产生的广泛争论需要进一步调查和实地测量,以了解草甘膦一旦分散在环境中的命运及其在食物链中的浓度。因此,需要该领域的分析师可以使用的经过验证的分析方法。在本次审查中,草甘膦及其主要代谢物的分析测定方法,AMPA,讨论,特别关注应用于谷物产品的色谱技术。实验程序进行了详细的解释,包括清理,衍生化,和仪器条件,为所涉及的实验室提供足够的信息,以继续实施这一分析线。常用的色谱方法是LC-MS/MS,GC-MS/SIM,和GC-MS/MS,但是,对于那些希望使用性能更好的高分辨率MS或更简单的HPLC-FLD的实验室,也有足够的适应症,HPLC-UV,GC-NPD,和用于筛选目的的GC-FPD技术。从文献中测得的小麦中草甘膦的浓度,玉米,大麦,黑麦,燕麦,大豆,据报道,谷物食品,以及它在世界各地的监管地位和积累机制。至于它在谷物中的积累,现有的数据表明,草甘膦倾向于积累更多的全麦面粉比在精制的,它在产品中的浓度严格取决于处理时间(越接近收获时间,浓度越高),在寒冷的气候下,除草剂往往会在土壤中长时间存在。
    The European Union\'s recent decision to renew the authorization for the use of glyphosate until 15 December 2033 has stimulated scientific discussion all around the world regarding its toxicity or otherwise for humans. Glyphosate is a chemical of which millions of tons have been used in the last 50 years worldwide to dry out weeds in cultivated fields and greenhouses and on roadsides. Concern has been raised in many areas about its possible presence in the food chain and its consequent adverse effects on health. Both aspects that argue in favor of toxicity and those that instead may indicate limited toxicity of glyphosate are discussed here. The widespread debate that has been generated requires further investigations and field measurements to understand glyphosate\'s fate once dispersed in the environment and its concentration in the food chain. Hence, there is a need for validated analytical methods that are available to analysts in the field. In the present review, methods for the analytical determination of glyphosate and its main metabolite, AMPA, are discussed, with a specific focus on chromatographic techniques applied to cereal products. The experimental procedures are explained in detail, including the cleanup, derivatization, and instrumental conditions, to give the laboratories involved enough information to proceed with the implementation of this line of analysis. The prevalent chromatographic methods used are LC-MS/MS, GC-MS/SIM, and GC-MS/MS, but sufficient indications are also given to those laboratories that wish to use the better performing high-resolution MS or the simpler HPLC-FLD, HPLC-UV, GC-NPD, and GC-FPD techniques for screening purposes. The concentrations of glyphosate from the literature measured in wheat, corn, barley, rye, oats, soybean, and cereal-based foods are reported, together with its regulatory status in various parts of the world and its accumulation mechanism. As for its accumulation in cereals, the available data show that glyphosate tends to accumulate more in wholemeal flours than in refined ones, that its concentration in the product strictly depends on the treatment period (the closer it is to the time of harvesting, the higher the concentration), and that in cold climates, the herbicide tends to persist in the soil for a long time.
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  • 文章类型: Journal Article
    曲马多等合成阿片类药物用于治疗轻度至中度疼痛。它缓解疼痛的能力约为吗啡的十分之一。此外,曲马多对5-羟色胺和去甲肾上腺素的作用与几种被称为5-羟色胺-去甲肾上腺素再摄取抑制剂(SNRIs)的抗抑郁药相似,如文拉法辛和度洛西汀。本文讨论了鉴定药物制剂和毒理学材料中药物的分析方法的最新进展,比如血,唾液,尿液,和头发。近年来,各种各样的分析仪器,包括毛细管电泳,NMR,紫外可见光谱,HPTLC,HPLC,LC-MS,GC,GC-MS,和电化学传感器,已用于药物制剂和毒理学样品中的药物鉴定。本研究重点介绍了当前用于各种矩阵中定量的主要定量技术。
    Synthetic opioids like Tramadol are used to treat mild to moderate pain. Its ability to relieve pain is about a tenth that of morphine. Furthermore, Tramadol shares similar effects on serotonin and norepinephrine to several antidepressants known as serotonin-norepinephrine reuptake inhibitors (SNRIs), such as venlafaxine and duloxetine. The present review paper discusses the recent developments in analytical methods for identifying drugs in pharmaceutical preparations and toxicological materials, such as blood, saliva, urine, and hair. In recent years, a wide variety of analytical instruments, including capillary electrophoresis, NMR, UV-visible spectroscopy, HPTLC, HPLC, LC-MS, GC, GC-MS, and electrochemical sensors, have been used for drug identification in pharmaceutical preparations and toxicological samples. The primary quantification techniques currently employed for its quantification in various matrices are highlighted in this research.
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