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液相色谱技术及液质联用技术在食品及农产品残留检测中的应用 总被引:6,自引:0,他引:6
讨论液相色谱相关技术及其在残留分析中的应用。介绍了用于样品前处理的固相提取技术(SPE)、液相色谱技术(HPLC)、液质联用技术(LC/MS)的特点,及其在食品及农产品中兽药、农药及毒素类有毒有害物质残留分析中的应用。 相似文献
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With the dramatic increase in the number of new chemical entities (NCEs) arising from combinatorial chemistry and modern high-throughput bioassays, novel bioanalytical techniques are required for the rapid determination of the metabolic stability and metabolites of these NCEs. Knowledge of the metabolic site(s) of the NCEs in early drug discovery is essential for selecting compounds with favorable pharmacokinetic credentials and aiding medicinal chemists in modifying metabolic \"soft spots\". In development, elucidation of biotransformation pathways of a drug candidate by identifying its circulatory and excretory metabolites is vitally important to understand its physiological effects. Mass spectrometry (MS) and nuclear magnetic resonance (NMR) have played an invaluable role in the structural characterization and quantification of drug metabolites. Indeed, liquid chromatography (LC) coupled with atmospheric pressure ionization (API) MS has now become the most powerful tool for the rapid detection, structure elucidation, and quantification of drug-derived material within various biological fluids. Often, however, MS alone is insufficient to identify the exact position of oxidation, to differentiate isomers, or to provide the precise structure of unusual and/or unstable metabolites. In addition, an excess of endogenous material in biological samples often suppress the ionization of drug-related material complicating metabolite identification by MS. In these cases, multiple analytical and wet chemistry techniques, such as LC-NMR, enzymatic hydrolysis, chemical derivatization, and hydrogen/deuterium-exchange (H/D-exchange) combined with MS are used to characterize the novel and isomeric metabolites of drug candidates. This review describes sample preparation and introduction strategies to minimize ion suppression by biological matrices for metabolite identification studies, the application of various LC-tandem MS (LC-MS/MS) techniques for the rapid quantification and identification of drug metabolites, and future trends in this field. 相似文献
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Anna Stachniuk Agata Sumara Magdalena Montowska Emilia Fornal 《Mass spectrometry reviews》2021,40(1):3-30
This review offers an overview of the current status and the most recent advances in liquid chromatography–mass spectrometry (LC‐MS) techniques with both high‐resolution and low‐resolution tandem mass analyzers applied to the identification and detection of heat‐stable species‐speci?c peptide markers of meat in highly processed food products. We present sets of myofibrillar and sarcoplasmic proteins, which turned out to be the source of 105 heat‐stable peptides, detectable in processed meat using LC‐MS/MS. A list of heat‐stable species‐specific peptides was compiled for eleven types of white and red meat including chicken, duck, goose, turkey, pork, beef, lamb, rabbit, buffalo, deer, and horse meat, which can be used as markers for meat authentication. Among the 105 peptides, 57 were verified by multiple reaction monitoring, enabling identification of each species with high specificity and selectivity. The most described and monitored species by LC‐MS/MS so far are chicken and pork with 26 confirmed heat‐stable peptide markers for each meat. In thermally processed samples, myosin, myoglobin, hemoglobin, l ‐lactase dehydrogenase A and β‐enolase are the main protein sources of heat‐stable markers. © 2019 John Wiley & Sons Ltd. Mass Spec Rev 相似文献
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Recent advances in mass spectrometry analysis of phenolic endocrine disruptors and related compounds
This article reviews recent literature on current methodologies based on chromatography coupled to mass spectrometry to analyze phenolic compounds with endocrine‐disrupting capabilities. For this review we chose alkylphenol ethoxylates, bisphenol A, bisphenol F, and their degradation products and halogenated derivatives, which are considered important environmental contaminants. Additionally, some related compounds such as bisphenol diglycidylethers were included. Growing attention has been paid to the mass spectrometric characterization of these compounds and the instrumentation and strategies used for their quantification and confirmation. The current use of gas chromatography–mass spectrometry (GC–MS) and liquid chromatography–mass spectrometry (LC–MS) methodologies with different mass spectrometers and ionization and monitoring modes is discussed. Practical aspects with regards to the use of these analytical techniques, such as derivatizing reagents in GC–MS, ion suppression in LC–MS, and the most problematic aspects of quantification, are included in the discussion. © 2009 Wiley Periodicals, Inc., Mass Spec Rev 29:776–805, 2010 相似文献
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采用LC/MS和LC-MS/MS法同时检测保健品中非法添加的伐地那非。用乙酸乙酯提取,以10 mmol•L-1的甲酸铵(pH 3.5)和乙腈为流动相,分别用Agilent Zorbax SB C18(150 mm×2.1 mm×5 μm)和Agilent Zorbax SB C18(100 mm×2.1 mm×3.5 μm)色谱柱分离,采用电喷雾离子源,正离子扫描方式进行分析检测。该方法简便、快捷、可靠,适用于保健品中非法添加伐地那非的常规检测。 相似文献
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The benefits of electrospray ionization are many, including sensitivity, robustness, simplicity and the ability to couple continuous flow methods with mass spectrometry. The technique has seen further improvement by lowering flow rates to the nanoelectrospray regime (<1,000 nL/min), where sample consumption is minimized and sensitivity increases. The move to nanoelectrospray has required a shift in the design of the electrospray source which has mostly involved the emitter itself. The emitter has seen an evolution in architecture as the shape and geometry of the device have proved pivotal in the formation of sufficiently small droplets for sensitive MS detection at these flow rates. There is a clear movement toward the development of emitters that produce multiple Taylor cones. Such multielectrospray emitters have been shown to provide enhanced sensitivity and sample utilization. This article reviews the development of nanoelectrospray emitters, including factors such as geometry and the manner of applying voltage. Designs for emitters that take advantage of multielectrospray are emphasized. © 2009 Wiley Periodicals, Inc., Mass Spec Rev 28:918–936, 2009 相似文献
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杀鼠药氟乙酰胺和氟乙酸钠LC/MS/MS分析 总被引:1,自引:0,他引:1
要建立了液质联用法(LC/MS/MS)测定杀鼠剂中氟乙酰胺和氟乙酸钠的方法。此二种药物由于具有价格便宜、合成简单、无色无味等特点,因此在中国被广泛非法使用。过去采用GCMS方法对其进行检测,但由于需要衍生化,所以费时费力,其衍生物也对测定产生干扰,本文采用LC/MS/MS方法同时对氟乙酰胺和氟乙酸钠进行了检测,方法快速、灵敏且不需要衍生化。 相似文献
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Recent advances in mycotoxin determination in food and feed by hyphenated chromatographic techniques/mass spectrometry 总被引:4,自引:0,他引:4
Mycotoxins are fungal toxins produced by molds, which occur universally in food and feed derivatives, and are produced under certain environmental conditions in the field before harvest, post-harvest, during storage, processing, and feeding. Mycotoxin contamination is one of the most relevant and worrisome problem concerning food and feed safety because it can cause a variety of toxic acute and chronic effects in human and animals. In this review we report the use of mass spectrometry in connection with chromatographic techniques for mycotoxin determination by considering separately the most diffuse class of mycotoxins: patulin, aflatoxins, ochratoxin A, zearalenone, trichothecenes, and fumonisins. Although the selectivity of mass spectrometry is unchallenged if compared to common GC and LC detection methods, accuracy, precision, and sensitivity may be extremely variable concerning the different mycotoxins, matrices, and instruments. The sensitivity issue may be a real problem in the case of LC/MS, where the response can be very different for the different ionization techniques (ESI, APCI, APPI). Therefore, when other detection methods (such as fluorescence or UV absorbance) can be used for the quantitative determination, LC/MS appears to be only an outstanding confirmatory technique. In contrast, when the toxins are not volatile and do not bear suitable chromophores or fluorophores, LC/MS appears to be the unique method to perform quantitative and qualitative analyses without requiring any derivatization procedure. The problem of exact quantitative determination in GC/MS and LC/MS methods is particularly important for mycotoxin determination in food, given the high variability of the matrices, and can be solved only by the use of isotopically labeled internal standards or by the use of ionization interfaces able to lower matrix effects and ion suppressions. When the problems linked to inconstant ionization and matrix effects will be solved, only MS detectors will allow to simplify more and more the sample preparation procedures and to avoid clean-up procedures, making feasible low-cost, high-throughput determination of mycotoxins in many different food matrices. 相似文献
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Metabolomics is a dynamically evolving field, with a major application in identifying biomarkers for drug development and personalized medicine. Numerous metabolomic studies have identified endogenous metabolites that, in principle, are eligible for translation to clinical practice. However, few metabolomic‐derived biomarker candidates have been qualified by regulatory bodies for clinical applications. Such interruption in the biomarker qualification process can be largely attributed to various reasons including inappropriate study design and inadequate data to support the clinical utility of the biomarkers. In addition, the lack of robust assays for the routine quantification of candidate biomarkers has been suggested as a potential bottleneck in the biomarker qualification process. In fact, the nature of the endogenous metabolites precludes the application of the current validation guidelines for bioanalytical methods. As a result, there have been individual efforts in modifying existing guidelines and/or developing alternative approaches to facilitate method validation. In this review, three main challenges for method development and validation for endogenous metabolites are discussed, namely matrix effects evaluation, alternative analyte‐free matrices, and the choice of internal standards (ISs). Some studies have modified the equations described by the European Medicines Agency for the evaluation of matrix effects. However, alternative strategies were also described; for instance, calibration curves can be generated in solvents and in biological samples and the slopes can be compared through ratios, relative standard deviation, or a modified Stufour suggested approaches while quantifying mainly endogenous metabolitesdent t‐test. ISs, on the contrary, are diverse; in which seven different possible types, used in metabolomics‐based studies, were identified in the literature. Each type has its advantages and limitations; however, isotope‐labeled ISs and ISs created through isotope derivatization show superior performance. Finally, alternative matrices have been described and tested during method development and validation for the quantification of endogenous entities. These alternatives are discussed in detail, highlighting their advantages and shortcomings. The goal of this review is to compare, apprise, and debate current knowledge and practices in order to aid researchers and clinical scientists in developing robust assays needed during the qualification process of candidate metabolite biomarkers. © 2019 John Wiley & Sons Ltd. Mass Spec Rev 相似文献
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A sensitive liquid chromatography-electrospray ionization-tandem mass spectrometric(LC-MS/MS) method for determination of compound 8601, 8602, 8603 in plasma was developed. The plasma compound 8601, 8602, 8603 was extracted using a solid phase extraction(SPE), and the sample extract was injected onto the LC-MS/MS system. The limit of quantitation(LLOQ) for compound 8601, 8602, 8603 is 0.500 μg•L-1. This method can be applied to the quantitation compound 8601, 8602, 8603 in plasma. 相似文献
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Michel Wagner David Tonoli Emmanuel Varesio Gérard Hopfgartner 《Mass spectrometry reviews》2016,35(3):361-438
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Among the different disciplines covered by mass spectrometry, measurement of (13)C/(12)C isotopic ratio crosses a large section of disciplines from a tool revealing the origin of compounds to more recent approaches such as metabolomics and proteomics. Isotope ratio mass spectrometry (IRMS) and molecular mass spectrometry (MS) are the two most mature techniques for (13)C isotopic analysis of compounds, respectively, for high and low-isotopic precision. For the sample introduction, the coupling of gas chromatography (GC) to either IRMS or MS is state of the art technique for targeted isotopic analysis of volatile analytes. However, liquid chromatography (LC) also needs to be considered as a tool for the sample introduction into IRMS or MS for (13)C isotopic analyses of non-volatile analytes at natural abundance as well as for (13)C-labeled compounds. This review presents the past and the current processes used to perform (13)C isotopic analysis in combination with LC. It gives particular attention to the combination of LC with IRMS which started in the 1990's with the moving wire transport, then subsequently moved to the chemical reaction interface (CRI) and was made commercially available in 2004 with the wet chemical oxidation interface (LC-IRMS). The LC-IRMS method development is also discussed in this review, including the possible approaches for increasing selectivity and efficiency, for example, using a 100% aqueous mobile phase for the LC separation. In addition, applications for measuring (13)C isotopic enrichments using atmospheric pressure LC-MS instruments with a quadrupole, a time-of-flight, and an ion trap analyzer are also discussed as well as a LC-ICPMS using a prototype instrument with two quadrupoles. 相似文献
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GC/MS/MS和LC/MS/MS在现代农产品分析中的应用 总被引:1,自引:0,他引:1
介绍了食品安全的影响及食品中有害物质分析的特点,着重介绍了GC/MS/MS和LC/MS/MS法在食品中的农药残留和兽药残留的分析应用。 相似文献