Gas chromatography–mass spectrometry

气相色谱 - 质谱法
  • 文章类型: Journal Article
    氨基甲酸乙酯(EC)是一种过程污染物,可以在食品和饮料的发酵和加工过程中作为副产物形成。EC浓度升高主要与蒸馏酒有关,但是这种化合物在食品和饮料中的浓度也较低,包括面包,酱油,和酒。来自动物研究的证据表明EC是一种可能的人类致癌物。因此,一些政府机构已经确定了食品供应中欧共体的允许限值。这篇综述包括欧共体的形成机制,食品供应中EC的发生,和EC饮食暴露评估。将涵盖用于检测EC的当前分析方法,除了新兴技术,如纳米传感器和表面增强拉曼光谱。各种缓解方法已被用来保持EC浓度低于允许的限制,包括蒸馏,酶处理,和酵母基因工程。需要在这一领域进行更多的研究来完善缓解策略并开发快速检测食品供应中的EC的方法。
    Ethyl carbamate (EC) is a process contaminant that can be formed as a by-product during fermentation and processing of foods and beverages. Elevated EC concentrations are primarily associated with distilled spirits, but this compound has also been found at lower concentrations in foods and beverages, including breads, soy sauce, and wine. Evidence from animal studies suggests that EC is a probable human carcinogen. Consequently, several governmental institutions have established allowable limits for EC in the food supply. This review includes EC formation mechanisms, occurrence of EC in the food supply, and EC dietary exposure assessments. Current analytical methods used to detect EC will be covered, in addition to emerging technologies, such as nanosensors and surface-enhanced Raman spectroscopy. Various mitigation methods have been used to maintain EC concentrations below allowable limits, including distillation, enzymatic treatments, and genetic engineering of yeast. More research in this field is needed to refine mitigation strategies and develop methods to rapidly detect EC in the food supply.
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  • 文章类型: Journal Article
    Microplastic research is a rapidly developing field, with urgent needs for high throughput and automated analysis techniques. We conducted a review covering image analysis from optical microscopy, scanning electron microscopy, fluorescence microscopy, and spectral analysis from Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy, pyrolysis gas-chromatography mass-spectrometry, and energy dispersive X-ray spectroscopy. These techniques were commonly used to collect, process, and interpret data from microplastic samples. This review outlined and critiques current approaches for analysis steps in image processing (color, thresholding, particle quantification), spectral processing (background and baseline subtraction, smoothing and noise reduction, data transformation), image classification (reference libraries, morphology, color, and fluorescence intensity), and spectral classification (reference libraries, matching procedures, and best practices for developing in-house reference tools). We highlighted opportunities to advance microplastic data analysis and interpretation by (i) quantifying colors, shapes, sizes, and surface topologies with image analysis software, (ii) identifying threshold values of particle characteristics in images that distinguish plastic particles from other particles, (iii) advancing spectral processing and classification routines, (iv) creating and sharing robust spectral libraries, (v) conducting double blind and negative controls, (vi) sharing raw data and analysis code, and (vii) leveraging readily available data to develop machine learning classification models. We identified analytical needs that we could fill and developed supplementary information for a reference library of plastic images and spectra, a tutorial for basic image analysis, and a code to download images from peer reviewed literature. Our major findings were that research on microplastics was progressing toward the use of multiple analytical methods and increasingly incorporating chemical classification. We suggest that new and repurposed methods need to be developed for high throughput screening using a diversity of approaches and highlight machine learning as one potential avenue toward this capability.
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  • 文章类型: Case Reports
    OBJECTIVE: Illicit drug abuse has reached an epidemic level in the United States. Drug overdose has become the leading cause of injury-related deaths since 2008 due to the recent surge of opioid overdose by heroin, controlled prescription drugs, and nonmethadone synthetic opioids. Synthetic designer drugs such as synthetic cathinones (\"bath salts\") and synthetic cannabinoids (\"Spice\" and \"K2\") continue to emerge and attract recreational users.
    METHODS: The emergence of new drugs of abuse poses a steep challenge for clinical toxicology laboratories. Limited information about the emerging drugs and their metabolism, \"rebranding\" of the illicit drugs, and a lack of Food and Drug Administration-approved screening methods for these drugs contribute to this difficulty. Here we review detection methods that can aid in identifying emerging drugs of abuse.
    RESULTS: One promising approach is the utilization of untargeted drug screening by mass spectrometry. Historically, gas chromatography-mass spectrometry has been the gold standard.
    CONCLUSIONS: Liquid chromatography-tandem mass spectrometry and liquid chromatography-high-resolution mass spectrometry offer improved detection capability of new drugs with simplified sample preparation, making it the new standard.
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  • 文章类型: Journal Article
    The continually-evolving field of fire debris analysis presents challenges to examiners on a regular basis. This article combines an overview of the scientific literature with novel samples that illustrate the current issues faced by fire debris examiners. Unusual liquids that contradict current classification schemes are discussed, as are complex matrices with noteworthy interferences. The matrix effects range from inherent interferences to the degradation of ignitable liquids. Finally, non-routine analyses are discussed, including the analysis of vegetable and lubricating oils and novel ignition methods. Through open discussion of complex samples and individual experiences, the problems in fire debris analysis can be overcome, resulting in the production of accurate and authoritative information.
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  • 文章类型: Journal Article
    Eicosanoids are potent lipid mediators of inflammation and are known to play an important role in numerous pathophysiological processes. Furthermore, inflammation has been proven to be a mediator of diseases such as hypertension, atherosclerosis, Alzheimer\'s disease, cancer and rheumatoid arthritis. Hence, these lipid mediators have gained significant attention in recent years. This review focuses on chromatographic and mass spectrometric methods that have been used to analyze arachidonic acid and its metabolites in brain tissue. Recently published analytical methods such as LC-MS/MS and GC-MS/MS are discussed and compared in terms of limit of quantitation and sample preparation procedures, including solid phase extraction and derivatization. Analytical challenges are also highlighted.
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  • 文章类型: Journal Article
    硒是生物体正常细胞功能的基本要素。然而,硒的毒性浓度仅比必需浓度高3至5倍。环境水中存在的无机形式(主要是亚硒酸盐和硒酸盐)通常表现出比有机形式更高的毒性(高达40倍)。因此,测定水中低水平的不同无机硒是一个分析挑战。在确定硒物质之前,固相萃取已被用作分离和/或预浓缩技术,因为需要精确测量极低含量的水中硒物质。本文对已发表的使用固相萃取作为预浓缩程序的水样中无机硒形态形成方法进行了严格的评论。根据超过75个参考文献,用于此任务的不同物种形成策略已被强调和分类。还讨论了固相萃取吸附剂以及已开发的Se形态形成方法的性能和分析特征。
    Selenium is an essential element for the normal cellular function of living organisms. However, selenium is toxic at concentrations of only three to five times higher than the essential concentration. The inorganic forms (mainly selenite and selenate) present in environmental water generally exhibit higher toxicity (up to 40 times) than organic forms. Therefore, the determination of low levels of different inorganic selenium species in water is an analytical challenge. Solid-phase extraction has been used as a separation and/or preconcentration technique prior to the determination of selenium species due to the need for accurate measurements for Se species in water at extremely low levels. The present paper provides a critical review of the published methods for inorganic selenium speciation in water samples using solid phase extraction as a preconcentration procedure. On the basis of more than 75 references, the different speciation strategies used for this task have been highlighted and classified. The solid-phase extraction sorbents and the performance and analytical characteristics of the developed methods for Se speciation are also discussed.
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  • 文章类型: Journal Article
    持久性有机污染物(POPs)由于其持久性而成为主要的环境问题。远程运输,生物积累和对生物体的潜在不利影响。分析化学在持久性有机污染物的测量中起着至关重要的作用,并提供了有关其分布和环境变化的重要信息。在过去的二十年中,人们付出了很多努力来开发更快,更安全,这些污染物的更可靠、更灵敏的分析技术。自12年前通过关于持久性有机污染物的斯德哥尔摩公约以来,分析方法得到了广泛的发展。这篇综述文章介绍了环境和生物群样品中持久性有机污染物测定的最新分析技术和应用,并总结了提取,卤化持久性有机污染物的分离和仪器分析。此外,这项审查涵盖了SCPOPs分析的重要方面(例如脂质测定和质量保证/质量控制(QA/QC)),最后讨论了改进持久性有机污染物分析和潜在新持久性有机污染物的未来趋势。
    Persistent organic pollutants (POPs) are major environmental concern due to their persistence, long-range transportability, bio-accumulation and potentially adverse effects on living organisms. Analytical chemistry plays an essential role in the measurement of POPs and provides important information on their distribution and environmental transformations. Much effort has been devoted during the last two decades to the development of faster, safer, more reliable and more sensitive analytical techniques for these pollutants. Since the Stockholm Convention (SC) on POPs was adopted 12 years ago, analytical methods have been extensively developed. This review article introduces recent analytical techniques and applications for the determination of POPs in environmental and biota samples, and summarizes the extraction, separation and instrumental analyses of the halogenated POPs. Also, this review covers important aspects for the analyses of SC POPs (e.g. lipid determination and quality assurance/quality control (QA/QC)), and finally discusses future trends for improving the POPs analyses and for potential new POPs.
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  • 文章类型: Journal Article
    背景:塞内西奥的地上部分是布赫。-火腿.(菊科)在中医治疗各种疾病方面有着悠久的历史,比如细菌性腹泻,肠炎,结膜炎,和呼吸道感染。
    方法:通过分析次要来源,完成了对Senecioscandens的书目调查,包括中药植物经典,互联网(谷歌学者和百度学者),和全球接受的科学数据库(Pubmed,Scopus,WebofScience,SciFinder,和CNKI)。仔细研究了这些来源,以获取有关千里光在中药中使用的现有信息,植物化学,药理学,和毒理学。
    结果:千里光是一种具有攀援木本茎的药用植物。植物化学研究表明存在许多有价值的化合物,如类黄酮,生物碱,酚酸,萜烯,挥发油,类胡萝卜素,和微量元素。其中,PA是特征性的成分,adonifoline是Senecioscanens的指标成分之一。现代药理学研究表明,从千里光中分离出的提取物和化合物具有广泛的药理活性,包括消炎药,抗菌,抗钩端螺旋体病,保肝,抗感染性疾病,抗氧化剂,抗病毒,抗肿瘤,镇痛药,诱变,和毒理学活动。
    结论:植物化学和药理研究表明,植物提取物具有各种药理活性,可归因于各种黄酮类化合物的存在,酚酸,和生物碱。需要开发用于PA的定性和定量方法的较新技术,以获得更好的准确性和灵敏度。由于这种药用植物中存在的PA的毒性,不同国家和地区对塞内西奥丑闻的法律规定各不相同。在中国,2010年《中国药典》对Senecioscanens的PAs毒性分级标准没有很好的定义,西方国家对PAs也没有严格的统一要求。我们建议应根据一组标准重新评估SenecioScandens的使用,其中包括风险-收益分析和毒性作用的严重程度,临床和临床前数据,以确保安全使用,同时继续满足获取药用植物的需求。
    BACKGROUND: The aerial parts of Senecio scandens Buch.-Ham. (family Asteraceae) have a long history in traditional Chinese medicine as a treatment for various ailments, such as bacterial diarrhea, enteritis, conjunctivitis, and respiratory tract infections.
    METHODS: A bibliographic investigation of Senecio scandens was accomplished by analyzing secondary sources, including the Chinese Medicinal plantal Classics, the Internet (Google Scholar and Baidu Scholar), and scientific databases accepted worldwide (Pubmed, Scopus, Web of Science, SciFinder, and CNKI). These sources were scrutinized for available information about the uses of Senecio scandens in traditional Chinese medicine, phytochemistry, pharmacology, and toxicology.
    RESULTS: Senecio scandens is a medicinal plant with a climbing woody stem. Phytochemical studies have shown the presence of numerous valuable compounds, such as flavonoids, alkaloids, phenolic acids, terpenes, volatile oils, carotenoids, and trace elements. Among them, PAs are the characteristic constituents, adonifoline is one of the index ingredients of Senecio scandens. Studies in modern pharmacology have demonstrated that extracts and compounds isolated from Senecio scandens show a wide spectrum of pharmacological activities, including anti-inflammatory, antimicrobial, anti-leptospirosis, hepatoprotective, anti-infusorial, antioxidant, antiviral, antitumoral, analgesic, mutagenic, and toxicological activities.
    CONCLUSIONS: Phytochemical and pharmacological studies have demonstrated that the extracts of the plant possess various pharmacological activities that can be attributed to the presence of various flavonoids, phenolic acids, and alkaloids. Newer technologies for qualitative and quantitative methods of PAs need to be developed to obtain better accuracy and sensitivity. Due to the toxicity of PAs present in this medicinal plant, the regulations on PAs of Senecio scandens were varied among different countries and regions. In China, the PAs toxicity of Senecio scandens ranking criteria is not well defined in the Chinese Pharmacopoeia 2010, and there is no strict uniform requirement on the PAs in western countries. We propose that the use of Senecio scandens should be reevaluated based on a set of criteria, which includes risk-benefit analysis and severity of the toxic effects, clinical and preclinical data to ensure safe use while continuing to satisfy the need for access to the medicinal plant.
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  • 文章类型: Journal Article
    Mass spectrometric approaches have been fundamental to the identification of metabolites associated with steroid hormones, yet this topic has not been reviewed in depth in recent years. To this end, and given the increasing relevance of liquid chromatography-mass spectrometry (LC-MS) studies on steroid hormones and their metabolites, the present review addresses this subject. This review provides a timely summary of the use of various mass spectrometry-based analytical techniques during the evaluation of steroidal biomarkers in a range of human disease settings. The sensitivity and specificity of these technologies are clearly providing valuable new insights into breast cancer and cardiovascular disease. We aim to contribute to an enhanced understanding of steroid metabolism and how it can be profiled by LC-MS techniques.
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