Methods of analysis

分析方法
  • 文章类型: Journal Article
    背景:全球,化妆品的消费和使用呈指数增长。有害金属的存在引发了人们对其对人类健康的潜在长期影响的担忧。目的:这篇综述的主要目的是揭示不同化妆品样品中重金属浓度的存在和范围,以及各种作者用来分析评估文章中危险金属的仪器技术。方法:这项分析集中在16种出版物上,这些出版物测量了铅等重金属的含量,镉,铁,镍,铬,以及2012年至2020年期间发布的各种化妆品样品中的汞。结果:研究结果支持这些金属作为污染物或成分存在于化妆品中,两者都对健康造成重大危害。法规和可接受的限制因国家而异,这对化妆品行业来说是一个重大挑战。结论:因此,迫切需要标准化化妆品中这些有毒金属的可接受限值。仪器技术,如AAS,石墨炉,ICP-OES/ICP-AES,研究人员使用ICP-MS分析化妆品中的有毒金属。
    Background: Globally, the consumption and use of cosmetics have increased exponentially. The presence of hazardous metals raises worries about their potential long-term impacts on human health. Objective: This review\'s primary goal is to shed light on the presence and ranges of heavy metal concentrations in diverse cosmetic samples as well as the instrumental techniques used by various authors to analyse the hazardous metals in the articles under evaluation. Methodology: This analysis concentrated on 16 publications that measured the levels of heavy metals like lead, cadmium, iron, nickel, chromium, and mercury in various cosmetic samples that were published between the years 2012 and 2020. Results: The study\'s findings support the existence of these metals as pollutants or components in cosmetics, both of which pose substantial health hazards. The regulations and acceptable limits vary across different countries, which is a significant challenge for the cosmetic industry. Conclusion: Therefore, there is a pressing need to standardise the acceptable limits of these toxic metals in cosmetics. Instrumental techniques such as AAS, GFAAS, ICP-OES/ICP-AES, and ICP-MS were employed by Researchers to analyse the toxic metals in cosmetics.
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  • 文章类型: Editorial
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  • 文章类型: Journal Article
    一种用于定性和定量测定氨基和羧酸的高灵敏度方法,以及所研究溶液中的一些尿素和蛋氨酸循环代谢物,是presented。氨基酸的衍生物(酯化)是通过它们在3N盐酸的正丁醇溶液中在65℃下反应15分钟而获得的,羧酸的衍生物是通过它们与苯酚在乙酸乙酯中与3N盐酸在65℃下反应20分钟而获得的。使用HPLC-MS/MS方法进行测定单个代谢物的实验工作,包括创建分析化合物的光谱库及其定量测定。已经开发了多重方法,用于定量分析3-4个数量级的广泛浓度范围内的所需代谢物。基于具有三重四极杆(QQQ)的质量分析仪对碎片形成的多个反应进行动态监测的方法,开发了分析代谢物的方法。内源性代谢物的有效色谱分离在13分钟内进行。所分析的化合物的校准曲线在整个浓度范围内是稳定的,并且具有拟合低于经验水平的潜力。开发的方法和获得的实验数据对广泛的生物医学研究感兴趣,以及在各种病理条件下监测生物样品中内源性代谢物的含量。该方法对氨基酸的灵敏度极限为约4.8nM,对羧酸为约0.5μM。可以在单个样品中测试多达19个氨基和多达12个羧酸和约10个相关代谢物。
    A highly sensitive method for the qualitative and quantitative determination of amino- and carboxylic acids, as well as a number of urea and methionine cycle metabolites in the studied solutions, is presented. Derivatives (esterification) were obtained for amino acids by their reaction in a solution of 3 N of hydrochloric acid in n-butanol for 15 min at 65 °C and for carboxylic acids by their reaction with phenol in ethyl acetate with 3 N of hydrochloric acid for 20 min at 65 °C. Experimental work on the determination of individual metabolites was carried out using the HPLC-MS/MS method and included the creation of a library of spectra of the analyzed compounds and their quantitative determination. Multiplex methods have been developed for the quantitative analysis of the desired metabolites in a wide range of concentrations of 3-4 orders of magnitude. The approach to the analysis of metabolites was developed based on the method of the dynamic monitoring of multiple reactions of the formation of fragments for a mass analyzer with a triple quadrupole (QQQ). The effective chromatographic separation of endogenous metabolites was carried out within 13 min. The calibration curves of the analyzed compounds were stable throughout the concentration range and had the potential to fit below empirical levels. The developed methods and obtained experimental data are of interest for a wide range of biomedical studies, as well as for monitoring the content of endogenous metabolites in biological samples under various pathological conditions. The sensitivity limit of the methods for amino acids was about 4.8 nM and about 0.5 μM for carboxylic acids. Up to 19 amino- and up to 12 carboxy acids and about 10 related metabolites can be tested in a single sample.
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  • 文章类型: Journal Article
    氯雷他定,4-(8-氯-5,6-二氢-11H-苯并[5,6]环庚[1,2-b]吡啶-11-亚基)-1-哌啶羧酸乙酯,是一种具有长效作用的抗组胺药物,对外周H1受体的选择性有限。它被广泛用于预防过敏性疾病,如鼻炎慢性荨麻疹,和哮喘。本章讨论,通过对文献的批判性广泛回顾,氯雷他定的名称描述,公式,元素组成,外观,制备方法。该配置文件包含氯雷他定的物理化学性质,包括pKa值,溶解度和X射线粉末衍射。此外,它涉及傅里叶变换红外光谱,核磁共振谱和质谱对官能团和结构的确认。本章还包括药物的分析方法,如药典,滴定法,电化学,光谱学,色谱和毛细管电泳方法。本章还涵盖了药物的临床应用,例如其用途,剂量,ADME概况和作用机制。
    Loratadine, 4-(8-Chloro-5,6-dihydro-11H-benzo[5,6]cyclohepta[1,2-b]pyridin-11-ylidene)-1-piperidinecarboxylic acid ethyl ester, is an antihistamine drug with long-acting effects and has limited selectivity for peripheral H1 receptors. It is widely used for the prevention of allergic diseases such as rhinitis chronic urticaria, and asthma. This chapter discusses, by a critical extensive review of the literature, the description of loratadine in terms of its names, formulae, elemental composition, appearance, methods of preparation. The profile contains physicochemical properties of Loratadine, including pKa value, solubility and X-ray powder diffraction. In addition, it involves Fourier transform infrared spectrometry, nuclear magnetic resonance spectroscopy and mass spectroscopy for functional groups and structural confirmation of. The chapter also includes methods of analysis of the drug such as compendial, titrimetric, electrochemical, spectroscopic, chromatographic and capillary electrophoretic methods. The chapter also covers clinical applications of the drug such as its uses, doses, ADME profiles and mechanism of action.
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  • 文章类型: Journal Article
    达那唑的全面概况,描述了命名法,公式,元素组成,外观,介绍了用途和应用。该概况包含用于制备药物物质的方法,并概述了其各自的方案。药物的物理特性,包括溶解度,X射线粉末衍射图,差示扫描量热法,描述了热行为和光谱研究。用于分析原料药和/或包括药典的药物制剂中的原料药的方法,分光光度,报告了电化学和色谱方法。的稳定性,毒性,药代动力学,生物利用度,药物评估和监测,比较,药理学,此外,还对所涉及的原料药进行了几项汇编审查。最后,本简介的末尾列出了二百七十九个参考文献。
    A comprehensive profile of danazol describing the nomenclatures, formulae, elemental composition, appearance, uses and applications is presented. The profile contains the method which was utilized for the preparation of the drug substance and its respective scheme is outlined. The physical characteristics of the drug including the solubility, X-ray powder diffraction pattern, differential scanning calorimetry, thermal behavior and spectroscopic studies are described. The methods which were used for the analysis of the drug substance in bulk drug and/or in pharmaceutical formulations including the compendial, spectrophotometric, electrochemical and the chromatographic methods are reported. The stability, toxicity, pharmacokinetics, bioavailability, drug evaluation and monitoring, comparisons, pharmacology, in addition to several compiled reviews on the drug substance which were involved. Finally, two hundred and seventy-nine references are listed at the end of this profile.
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  • 文章类型: Journal Article
    长春西汀(VIN)是从长春花植物中提取的草药补充剂。它是一个多行动代理,用于治疗各种神经系统疾病,如阿尔茨海默病和帕金森病。长春西汀也有抗炎作用,镇痛药,抗氧化性能和治疗各种思维和记忆问题。目前,长春西汀也可在市场上作为膳食补充剂,以增强认知和记忆。这个配置文件解释了物理化学性质,制备方法,长春西汀的相关杂质含量和不同的光谱行为。它还讨论了报告的药物分析方法,其中包括Compendial方法,电化学方法,分光光度法和色谱分析方法。此外,这个配置文件解释了药物在酸胁迫条件下的稳定性,碱性和光解降解。此外,该药物的临床应用,其用途,副作用,剂量信息,还讨论了药代动力学和作用机理。
    Vinpocetine (VIN) is a herbal supplement extracted from the periwinkle plant. It is a multi-action agent, which is used to treat various neurological disorders such as Alzheimer\'s and Parkinson\'s disease. Vinpocetine has also anti-inflammatory, analgesic, antioxidant property and treats various thinking and memory problems. Currently, vinpocetine is also available in the market as a dietary supplement to enhance cognition and memory. This profile explains the physicochemical properties, methods of preparation, content of related impurities and different spectroscopical behavior of vinpocetine. It also discusses the reported methods of analysis of the drug, which include Compendial Methods, Electrochemical Methods, Spectrophotometric Methods and Chromatographic Methods of analysis. Furthermore, this profile explains the stability of the drug subjected to stress conditions of acid, alkaline and photolytic degradation. In addition, the clinical applications of the drug, its uses, side effects, dosing information, pharmacokinetics and mechanism of action are also discussed.
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  • 文章类型: Journal Article
    在过去的二十年中,常规监管监测中的海洋生物毒素分析在欧洲(EU)和其他地区已从使用小鼠生物测定法(MBA)向高端分析技术如高效液相色谱(HPLC)和串联质谱(MS)取得了显着进展。以前,接受这些先进的方法,在远离MBA的过程中,由于缺乏用于方法开发和验证的商业认证分析标准而受到阻碍。现在已经解决了这一问题,欧盟几家公司提供了广泛的分析标准,北美和亚洲加强了方法的开发和验证,以达到所需的监管标准。然而,高端分析设备的成本,对于常规监测实验室来说,冗长的程序和需要合格人员进行分析仍然是一个挑战。在发展中地区,水产养殖产量正在增加,替代廉价的敏感,可测量,适用于新手最终用户的准确和实时(SMART)快速现场测试(POST)方法,可以进行验证并获得国际认可,这仍然是监管机构和行业的目标。市场上用于海洋毒素分析的商业检测试剂盒的范围仍然有限,尤其是那些符合监管控制要求的试剂盒。单独的测定包括酶联免疫吸附测定(ELISA)和基于侧流膜的免疫测定(LFIA),用于欧盟调节的毒素,如冈田酸(OA)和双植物毒素(DTX),3种不同的测试形式的毒素(STX)及其类似物和软骨瘤酸(DA),为行业提供不同的成本和收益。从文献中可以观察到,这些测定不仅正在进行发展和改进,但也有新的检测正在开发使用国家的最先进的生物传感器技术。这篇综述侧重于目前可用的方法和海洋生物毒素测试创新方法的最新进展,以及需要观察的最终用户实用性。此外,它强调了影响测定发展的趋势,如多路复用能力和快速开机自检,表明将塑造未来市场的潜在检测方法。
    In the past twenty years marine biotoxin analysis in routine regulatory monitoring has advanced significantly in Europe (EU) and other regions from the use of the mouse bioassay (MBA) towards the high-end analytical techniques such as high-performance liquid chromatography (HPLC) with tandem mass spectrometry (MS). Previously, acceptance of these advanced methods, in progressing away from the MBA, was hindered by a lack of commercial certified analytical standards for method development and validation. This has now been addressed whereby the availability of a wide range of analytical standards from several companies in the EU, North America and Asia has enhanced the development and validation of methods to the required regulatory standards. However, the cost of the high-end analytical equipment, lengthy procedures and the need for qualified personnel to perform analysis can still be a challenge for routine monitoring laboratories. In developing regions, aquaculture production is increasing and alternative inexpensive Sensitive, Measurable, Accurate and Real-Time (SMART) rapid point-of-site testing (POST) methods suitable for novice end users that can be validated and internationally accepted remain an objective for both regulators and the industry. The range of commercial testing kits on the market for marine toxin analysis remains limited and even more so those meeting the requirements for use in regulatory control. Individual assays include enzyme-linked immunosorbent assays (ELISA) and lateral flow membrane-based immunoassays (LFIA) for EU-regulated toxins, such as okadaic acid (OA) and dinophysistoxins (DTXs), saxitoxin (STX) and its analogues and domoic acid (DA) in the form of three separate tests offering varying costs and benefits for the industry. It can be observed from the literature that not only are developments and improvements ongoing for these assays, but there are also novel assays being developed using upcoming state-of-the-art biosensor technology. This review focuses on both currently available methods and recent advances in innovative methods for marine biotoxin testing and the end-user practicalities that need to be observed. Furthermore, it highlights trends that are influencing assay developments such as multiplexing capabilities and rapid POST, indicating potential detection methods that will shape the future market.
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  • 文章类型: Journal Article
    There are many technical and nontechnical steps involved in a successful clinical functional MRI (fMRI) scan. The output from scanning and analysis can only be as good as the input, so task instruction and rehearsal are the most important steps during an clinical fMRI procedure. Properly pre-processed data significantly affects statistical analysis, which has a great impact on image interpretation. Even though there is general agreement on how to process clinical fMRI data, such as algorithms for head motion detection and correction, the theory and practicalities associated with data processing remain complex and constantly evolving.
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  • 文章类型: Journal Article
    恩曲他滨(Emtriva,FTC)是一种抗病毒药物,可减少人体的HIV含量。抗HIV药物的恩曲他滨减缓或保护免疫系统免受损害,并降低与AIDS发展相关的疾病的风险。恩曲他滨也用于治疗乙型肝炎病毒。恩曲他滨是一类被称为核苷逆转转录酶抑制剂(NRTIs)的药物。鉴于恩曲他滨的临床意义,对药物和生物系统中用于测试药物的多种分析技术的物理和药物特性以及细节进行了全面审查。调查的方法包括鉴定试验,光谱学,色谱,电化学,和热。除了分析配置文件之外,恩曲他滨的降解和稳定性,其药理学和药代动力学,制药应用,行动机制,剂型和剂量,ADME配置文件,和互动一直在争论。
    Emtricitabine (Emtriva, FTC) is an antiviral medicine which decreases the body\'s amount of HIV. Emtricitabine on of Anti-HIV drugs slow down or protect the immune system against damage and reduce the risk of diseases related to developing of AIDS. Emtricitabine use also for treatment of hepatitis B virus. Emtricitabine is a drug class known as nucleoside reversing transcriptase inhibitors (NRTIs). In view of Emtricitabine\'s clinical significance, a thorough review of the physical and pharmaceutical characteristics and details of the multiple analytical techniques used to test the drug in pharmaceutical and biological systems was conducted. The methods investigated include identification test, Spectroscopy, chromatography, electrochemicals, and Thermal. Beside the analytical profile, the degradation and stability of Emtricitabine, its pharmacology and pharmacokinetics, Pharmaceutical Applications, Mechanism of Action, dosage forms and dose, ADME profile, and interactions have been debated.
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  • 文章类型: Journal Article
    吡罗昔康的全面概况,包括命名法,公式,元素组成,外观,用途和应用。概述了用于制备药物的方法及其各自的方案。药物的物理特性包括电离常数,溶解度,x射线粉末衍射图,差示扫描量热法,描述了热行为和光谱研究。用于分析原料药和/或包括药典的药物制剂中的原料药的方法,分光光度,报告了电化学和色谱方法。的稳定性,毒性,药代动力学,生物利用度,药物评价,比较,除了收集有关原料药的评论外,还涉及。最后,在此配置文件的末尾列出了四百五十多个参考文献。
    A comprehensive profile of piroxicam including the nomenclatures, formulae, elemental composition, appearance, uses and applications. The methods which were utilized for the preparation of the drug substance and their respective schemes are outlined. The physical characteristics of the drug including the ionization constant, solubility, x-ray powder diffraction pattern, differential scanning calorimetry, thermal behavior and spectroscopic studies are described. The methods which were used for the analysis of the drug substance in bulk drug and/or in pharmaceutical formulations including the compendial, spectrophotometric, electrochemical and the chromatographic methods are reported. The stability, toxicity, pharmacokinetics, bioavailability, drug evaluation, comparison, in addition to compiled reviews on the drug substance are involved. Finally, more than four hundred and fifty references are listed at the end of this profile.
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