Determination

Determination
  • 文章类型: Journal Article
    尽管茶叶广泛用作新烟碱类,但对茶叶中氮吡喃的测定和行为的研究仍然有限。建立了一种专门用于检测茶叶中硝啶的有机节省分析方法。通过沸水提取Nitenpyra,并用CleanertPCX固相净化。平均回收率为75.1-94.5%,相对标准偏差(RSD)为0.7-8.6%,可节省34.5-88.6%的有机溶剂。新鲜茶芽中的定量限(LOQs)为0.002mg·kg-1,制茶中含有0.005mg·kg-1,和0.001mg·L-1在茶水中,满足当前最小最大残留限制(MRL)。在推荐剂量(27ga.i.ha-1)下,Nitenpyra在两个位置迅速消散,半衰期为1.2-1.4天。值得注意的是,在不同的冲泡模式下,从制成的茶中浸出20-110%的氮吡喃。这项工作提供了有关nitenpyra在茶叶种植中的合理应用的见解,并为负责茶叶中未建立的MRL的机构提供了考虑。
    Studies on nitenpyram determination and behavior within tea remain limited despite its widespread use as a neonicotinoid. An organic-saving analytical approach tailored for the detection of nitenpyram in tea was established. Nitenpyram was extracted by boiling water and cleaned up by Cleanert PCX solid-phase. The average recoveries were 75.1-94.5 %, with relative standard deviations (RSDs) of 0.7-8.6 % for saving 34.5-88.6 % organic solvent. The limits of quantification (LOQs) were 0.002 mg·kg-1 in fresh tea shoots, 0.005 mg·kg-1 in made tea, and 0.001 mg·L-1 in tea brew, satisfying the current minimum Maximum Residue Limit (MRL). Nitenpyram dissipated rapidly with half-lives of 1.2-1.4 days at the recommended dosage (27 g a.i. ha-1) in two locations. Remarkably, 20-110 % of nitenpyram was leached out from made tea in different brewing modes. This work provides insights into nitenpyram\'s rational application in tea cultivation and offers considerations to institutions tasked with unestablished MRLs in tea.
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  • 文章类型: Journal Article
    检测白酒中糠醛的浓度可用于评价白酒的质量,允许优化加工技术和提高整体质量。在本文中,开发了一种基于碳点(o-CD)的荧光增强方法,用于测定中国白酒中的糠醛。在充满·SO4-和·OH的环境中,糠醛与o-CD上的邻二氨基发生直接表面反应。产生的呋喃基咪唑增加了表面电子密度,导致发射增强和颜色从橙色变为绿色。因此,在水中建立o-CD-TA对糠醛的线性荧光响应,检测极限为30.5nM。最后,乙醇校正后,用于测定白酒中的糠醛,具有较高的精密度和重现性,提供一种低成本、高灵敏度的新策略。特别是,通过自由基的帮助将目标分子共价连接到CD表面的想法开辟了一条新的途径,通过将化学作用实现碳纳米结构来合并纳米级和分子领域。
    Detecting the furfural concentration in Baijiu can be used to assess the quality of Baijiu, allowing for the optimization of processing techniques and the enhancement of overall quality. In this paper, a fluorescence-enhanced method based on carbon dots (o-CDs) is developed for the furfural determination in Chinese Baijiu. In an environment full-filled with ·SO4- and ·OH, furfural undergone a direct surface reaction with the ortho-diamino groups at o-CDs. The created furan-based imidazole increased the surface electron density, leading an emission enhancement and color changes from orange to green. Thereby, a linear fluorescence response of o-CDs-TA to furfural is established in water with a detection limit of 30.5 nM. Finally, after ethanol correction it is used to determine furfural in Chinese Baijiu with high precision and reproducibility, providing a new strategy with low-cost and high sensitivity. In particular, the idea of covalently connecting target molecule to the CDs surface via the assistance of free radical opens a new avenue to merge the nanoscale and molecular realms through implementing chemical role into carbon nanostructures.
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  • 文章类型: Journal Article
    木质素是一种坚韧的生物聚合物,可赋予植物力量和保护作用。这也是将植物生物质转化为生物燃料的主要障碍,因为它阻止酶进入富含糖的纤维。为了优化生物燃料生产,我们需要准确有效地测量植物组织中的木质素含量。在这个协议中,我们描述了一种简单可靠的方法来测量植物组织中的总木质素含量。该方法使用乙酰溴,一种将木质素溶解成可溶性衍生物的化学物质,可以通过它们在280nm处的吸光度来检测它们。该方法包括两个步骤:首先,我们从植物样本中获得了脱淀粉细胞壁材料,第二,我们用乙酰溴处理细胞壁材料并测量木质素溶液的吸光度。该方法可以捕获所有类型的木质素,并且对不同的植物组织效果很好。
    Lignin is a tough biopolymer that gives plants strength and protection. It is also a major obstacle for converting plant biomass into biofuels because it prevents enzymes from accessing the sugar-rich fibers. To optimize biofuel production, we need to measure the lignin content in plant tissues accurately and efficiently. In this protocol, we describe a simple and reliable method to measure the total lignin content in plant tissues. The method uses acetyl bromide, a chemical that dissolves lignin into soluble derivatives and makes it possible to detect them by their absorbance at 280 nm. The method consists of two steps: first, we obtained destarched cell wall material from the plant samples, and second, we treat the cell wall material with acetyl bromide and measure the absorbance of the lignin solution. This method can capture all types of lignin and works well with different plant tissues.
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  • 文章类型: Journal Article
    目标:一个新的,开发了选择性和简单的UPLC-MS/MS方法,并对其进行了验证,用于测定人血浆和泪液中的lifitegrast,以获得PK数据。材料和方法:在样品中加入Lifitegrast-d4溶液,然后提取并转移到UPLC小瓶中。结果:各自的工作范围在血浆中为25.00-2000.00μg/ml,在泪液中为4.00-1000.00μg/ml。经过充分验证的方法符合现有的准确性和精密度监管标准,recovery,等。它适用于血浆和泪液样本,来自一项临床研究,成功。结论:该方法可用于血浆和泪液中lifitegrast的评估。
    [方框:见正文]。
    Aim: A new, selective and simple UPLC-MS/MS method was developed and validated for the determination of lifitegrast in human plasma and tear in order to obtain PK data. Materials & methods: Lifitegrast-d4 solutions were added in the samples, and then were extracted and transferred to a UPLC vial. Results: The respective working ranges were 25.00-2000.00 pg/ml in plasma and 4.00-1000.00 μg/ml in tear. The fully validated method complied with existing regulatory criteria for accuracy and precision, recovery, etc. It was applied to plasma and tear samples, which were from a clinical study, successfully. Conclusion: This method is useful in the evaluation of lifitegrast in plasma and tear.
    [Box: see text].
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  • 文章类型: Journal Article
    苯醚甲环唑的耗散行为和最终残留水平,丙草胺,丙环唑,使用田间试验和实验室测定研究了无花果中的吡唑酮酯。三因素,设计了三水平正交试验来优化该方法的预处理条件。建立了高效液相色谱-串联质谱法测定苯醚甲环唑的方法,丙草胺,丙环唑,和无花果中的吡唑醚酯残留物。无花果中所有四个靶标的定量极限为0.002mg/kg。苯醚环唑,丙草胺,丙环唑,在无花果中,吡唑酯是易消化的农药,半衰期为6.4、6.2、4.8和7.9天,分别。苯醚甲环唑的残留,丙草胺,丙环唑,无花果中的吡唑酮酯低于欧盟确定的0.1、0.03、0.01和0.02mg/kg的残留水平,分别,应用后第7天。吡唑酮,丙环唑,苯醚甲环唑,和丙草胺以75、125、150和200mga.i./kg的剂量以7天的间隔施用两次,最后一次施用后7天,无花果中四种杀菌剂的残留物是可以接受的。因此,根据方案,70%苯醚甲环唑-丙氯醚可湿性粉剂和40%吡唑酮-丙环唑水性乳剂的安全间期可设定为7天.
    Dissipative behavior and final residue levels of difenoconazole, prochloraz, propiconazole, and pyraclostrobin in figs were investigated using field trials and laboratory assays. A three-factor, three-level orthogonal test was designed to optimize the pretreatment conditions of the method. A method was established using high-performance liquid chromatography tandem mass spectrometry for the determination of difenoconazole, prochloraz, propiconazole, and pyraclostrobin residues in figs. The limit of quantification for all four targets in figs was 0.002 mg/kg. Difenoconazole, prochloraz, propiconazole, and pyraclostrobin are readily digestible pesticides in figs with half-lives of 6.4, 6.2, 4.8, and 7.9 days, respectively. Residues of difenoconazole, prochloraz, propiconazole, and pyraclostrobin in figs were below the European Union established residue levels of 0.1, 0.03, 0.01, and 0.02 mg/kg, respectively, at day 7 after application. Pyraclostrobin, propiconazole, difenoconazole, and prochloraz were applied twice at doses of 75, 125, 150, and 200 mg a.i./kg at 7-day intervals, and the residues of the four fungicides in figs were acceptable 7 days after the last application. Therefore, the safety interval can be set at 7 days for 70% difenoconazole-prochloraz wettable powder and 40% pyraclostrobin-propiconazole aqueous emulsion according to the protocol.
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  • 文章类型: Journal Article
    人们经常服用替扎尼定(TIZ)来治疗由多发性硬化症或脊髓损伤等疾病引起的痉挛。它还有助于防止肌肉痉挛。它通过抑制大脑和脊髓中的特定神经信号,有助于放松和释放紧张和僵硬的肌肉。本研究中采用的技术利用了苯并呋喃在特定条件下与TIZ反应时赋予荧光特性的独特能力。这种荧光特性被用来进化出一种非常敏感的,负担得起的,和定量TIZ的选择性方法。所得黄色荧光产物在波长532.9nm处观察到,并且施加474.9nm的激发波长光束。通过观察整个TIZ浓度的反应,在40-500ng/mL范围内评估校准图的线性。通过计算,该方法的检测水平(LOD)被确定为11.9ng/mL,而定量水平约为36ng/mL。对影响该策略疗效的所有相关因素进行了彻底检查和相应调整。建议的策略按照ICH概述的指南进行了验证。结果证实了该方法对片剂中TIZ的准确定量的能力,加标血浆,和药物评估含量均匀性。
    People frequently administer Tizanidine (TIZ) to treat spasticity resulting from diseases like multiple sclerosis or spinal cord injuries. It also helps prevent muscle spasms. It helps to relax and release tense and stiff muscles by inhibiting specific nerve signals in the brain and spinal cord. The technique employed in this study made use of the unique ability of benzofurazan to confer fluorescent character when reacted with TIZ at specific conditions. This fluorogenic property was harnessed to evolve a remarkably sensitive, affordable, and selective method to quantify TIZ. The resulting yellow fluorescent product was observedat a wavelength beam of 532.9 nm, and an excitation wavelength beam of 474.9 nm was applied. By looking at the response across the TIZ concentration, the calibration chart\'s linearity was assessed in the range of 40-500 ng/mL. By computation, the approach\'s detection level (LOD) was determined to be 11.9 ng/mL, while the quantitation level was approximated to be 36 ng/mL. All pertinent factors impacting the strategy\'s efficacy were thoroughly inspected and adjusted accordingly. The proposed strategy was validated following the guidelines outlined by the ICH. The outcomes confirmed the method\'s capability for the accurate quantifying of TIZ in tablets, spiked plasma, and pharmaceutical assessing content uniformity.
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  • 文章类型: Journal Article
    新烟碱,作为增长最快的一类杀虫剂,目前占全球农药市场的25%以上。它们在控制对农田构成威胁的各种害虫方面的有效性,家庭院子/花园,不能否认高尔夫球场果岭。然而,新烟碱的广泛使用导致传粉者等非靶标生物的显着下降,昆虫,和鸟。此外,潜在的慢性,这些化合物对人体健康的亚致死效应在很大程度上仍是未知的。为了解决这些紧迫的问题,探索和了解电化学传感器在检测新烟碱残留方面的能力至关重要。令人惊讶的是,尽管这个话题越来越重要,目前文献中没有全面的评论文章。因此,我们提出的综述旨在通过全面分析使用电化学方法测定新烟碱来弥补这一差距.在这篇评论文章中,我们将深入研究电化学分析的各个方面,包括电极材料的影响,采用的技术,和使用不同类型的电极机构。通过综合和分析该领域的现有研究,我们的审查将为研究人员提供有价值的见解和指导,科学家,和政策制定者一样。
    Neonicotinoids, as the fastest-growing class of insecticides, currently account for over 25% of the global pesticide market. Their effectiveness in controlling a wide range of pests that pose a threat to croplands, home yards/gardens, and golf course greens cannot be denied. However, the extensive use of neonicotinoids has resulted in significant declines in nontarget organisms such as pollinators, insects, and birds. Furthermore, the potential chronic, sublethal effects of these compounds on human health remain largely unknown. To address these pressing issues, it is crucial to explore and understand the capabilities of electrochemical sensors in detecting neonicotinoid residues. Surprisingly, despite the increasing importance of this topic, no comprehensive review article currently exists in the literature. Therefore, our proposed review aims to bridge this gap by providing a thorough analysis of the use of electrochemical methods for neonicotinoid determination. In this review article, we will delve into various aspects of electrochemical analysis, including the influence of electrode materials, employed techniques, and the different types of electrode mechanisms utilized. By synthesizing and analysing the existing research in this field, our review will offer valuable insights and guidance to researchers, scientists, and policymakers alike.
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  • 文章类型: Journal Article
    铊(Tl)是一种潜在的毒性元素,具有重大的生态和环境风险。最近,大量的Tl通过自然和人类活动释放到环境中,这引起了越来越多的关注。这种有害和微量元素的测定对于控制其污染至关重要。本文总结了优化Tl检测技术的进步和进展,包括原子吸收光谱(AAS),伏安法,基于电感耦合等离子体(ICP)的方法,分光光度法,和基于X射线的方法。此外,它介绍了采样和预处理方法,如薄膜中的扩散梯度(DGT),液-液萃取,固相萃取,和浊点提取。在这些技术中,ICP-质谱(MS)是Tl检测的优选选择,这是由于其在确定Tl及其种类和同位素组成方面的高精度。同时,一些新的材料和试剂被用于检测。讨论了新型工作电极材料和显色剂的应用。重点放在减少溶剂消耗和利用预处理技术,如超声辅助工艺和功能化的磁性颗粒。大多数检测是在水性基质中进行的,同时总结了应用于固相的基于X射线的方法,这些方法提供了无损分析。这项工作提高了对Tl测定技术的理解,同时为寻求适当分析技术的研究人员提供了宝贵的资源。
    Thallium (Tl) is a potential toxicity element that poses significant ecological and environmental risks. Recently, a substantial amount of Tl has been released into the environment through natural and human activities, which attracts increasing attention. The determination of this hazardous and trace element is crucial for controlling its pollution. This article summarizes the advancement and progress in optimizing Tl detection techniques, including atomic absorption spectroscopy (AAS), voltammetry, inductively coupled plasma (ICP)-based methods, spectrophotometry, and X-ray-based methods. Additionally, it introduces sampling and pretreatment methods such as diffusive gradients in thin films (DGT), liquid-liquid extraction, solid phase extraction, and cloud point extraction. Among these techniques, ICP-mass spectrometry (MS) is the preferred choice for Tl detection due to its high precision in determining Tl as well as its species and isotopic composition. Meanwhile, some new materials and agents are employed in detection. The application of novel work electrode materials and chromogenic agents is discussed. Emphasis is placed on reducing solvent consumption and utilizing pretreatment techniques such as ultrasound-assisted processes and functionalized magnetic particles. Most detection is performed in aqueous matrices, while X-ray-based methods applied to solid phases are summarized which provide non-destructive analysis. This work improves the understanding of Tl determination technology while serving as a valuable resource for researchers seeking appropriate analytical techniques.
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  • 文章类型: Journal Article
    高干扰和应用范围窄是目前荧光分析方法的瓶颈,限制了其在传感领域的广泛应用。因此,为了克服这些缺点,在这项工作中,首次构建了利用小檗碱(BER)和二氢硫辛酸(DHLA-AgNCs)保护的银纳米簇的比率荧光传感系统,实现BER和柔红霉素(Dau)的测定。BER水溶液(非平面构象)没有荧光发射。当它与DHLA-AgNCs混合时,BER的构象变成了平面,除了DHLA-AgNCs在653nm处的荧光发射峰之外,还在515nm处产生荧光发射。随着系统中BER浓度的增加,515nm处BER(平面构象)的荧光强度明显增加,DHLA-AgNCs的荧光强度略有下降。因此,构建了基于荧光物质和非荧光物质的双发射荧光传感系统,实现BER的测定。同时,基于BER的桥接效应和Dau的荧光共振能量转移效应,利用两个峰强度的改变来实现Dau的测定。因此,这种双发射传感系统不仅可以用于BER及其类似物的荧光分析,但也基于误码率的桥接效应,允许测定不能用银纳米团簇直接测量的Dau及其类似物,拓展了传统双排放检测系统的应用范围。同时,该系统抗干扰能力强,对人体毒性低,对样品和环境污染少。这为今后新型荧光传感系统的构建提供了新的方向和普适性的研究策略,用于常规荧光分析方法无法直接检测的目标物质的分析。
    High interference and narrow application range are key of bottleneck of recent fluorescence analysis methods, which limit their wide application in the sensing field. Therefore, to overcome these disadvantages, a ratiometric fluorescence sensing system utilizing berberine (BER) and silver nanoclusters protected by dihydrolipoic acid (DHLA-AgNCs) was constructed for the first time in this work, to achieve determination of BER and daunorubicin (Dau). BER aqueous solution (non-planar conformation) has no fluorescence emission. When it was mixed with DHLA-AgNCs, the conformation of BER became planar, producing fluorescence emission at 515 nm besides the fluorescence emission peak of DHLA-AgNCs at 653 nm. With the increase of BER concentration added in system, the fluorescence intensity of BER (planar conformation) at 515 nm increased obviously and the fluorescence intensity of DHLA-AgNCs decreased slightly. Therefore, the dual emission fluorescence sensing system was constructed based on a fluorescence substance and non fluorescence substance, to achieve determination of BER. Meanwhile, based on the bridging effect of BER and fluorescence resonance energy transfer effect from Dau, the altering of two peaks intensity was utilized to achieve determination of Dau. Thus, this dual emission sensing system can not only be used for fluorescence analysis of BER and its analogues, but also based on the bridging effect of BER, allowing the determination of Dau and its analogues that could not be directly measured with silver nanoclusters, expanding the application range of traditional dual emission detection systems. Meanwhile, this system has strong anti-interference ability and low toxicity to the human body and less pollution to the sample and environment. This provides a new direction and universal research strategy for the construction of new fluorescence sensing systems in the future for the analysis of target substances that cannot be directly detected with conventional fluorescence analysis methods.
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  • 文章类型: Journal Article
    作为铀系列的衰变产物,210Pb在自然界中广泛传播,并具有很强的放射性和化学毒性。建立可靠有效的210Pb放射分析方法以支持环境和食品放射性监测计划至关重要。本文批判性地回顾了用于测定环境和生物样品中210Pb的分析方法,尤其是近年来的新发展。在不同分析步骤中应用的技术,包括样品预处理,分离,净化,总结和检测,并讨论了它们的利弊,为210Pb环境和生物测定提供了一个整体概述。
    As a decay product of uranium series, 210Pb spreads widely in the nature and imposes strong radiological and chemical toxicity. It is vital to establish reliable and efficient radioanalytical methods for 210Pb determination to support environment and food radioactivity monitoring programs. This article critically reviews analytical methods developed for determining 210Pb in environmental and biological samples, especially new development in recent years. Techniques applied throughout different analytical steps including sample pretreatment, separation, purification, and detection are summarized and their pros and cons are discussed to provide a holistic overview for 210Pb environmental and biological assay.
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