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Rapid Analysis of Flavors and Fragrances Using High-Efficiency GC ColumnsThere are many misconceptions about what it means to perform fast gas chromatography (GC) and what the term fast GC implies. Fast GC is often associated with the use of hydrogen as a carrier gas and, although this is certainly a good approach, it is not always necessary to shorten the analysis time. A second misconception is that changing column dimension results in time-consuming method development. Using high-efficiency GC columns can greatly reduce the analysis time and when coupled with the method translation software, the time spent on method development can be greatly minimized.
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Improving on GC–MS Performance for Demanding Applications: The Use of GC Coupled to Tandem-Quadrupole MSGas chromatography–mass spectrometry (GC–MS) and liquid chromatography (LC)–MS are widespread successful approaches, based on single-quadrupole MS, for the routine detection, identification, and quantitation of compounds. There has, however, been increasing interest in the use of tandem MS in more challenging, complex matrices such as those commonly found in food, environmental, and biological analyses. The combination of GC with tandem-quadrupole MS (MS-MS) is discussed, where the inherent increase in selectivity and sensitivity of the approach has enabled rapid, confident compound detection and quantitation for such demanding applications.
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Use of an Efficient LC Method Development Approach in the Analysis of Terfenadine, Fexofenadine and AzaclonolUsing ACQUITY UPLC technology with triple quadrupole MS detection enhances the selectivity, sensitivity and throughput in quantitative bioanalytical studies. Detection limits for these methods are being driven lower and lower as drugs become more potent.
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Multimodal HPLC Screening of Polysaccharide-based Chiral Stationary PhasesHigh-performance liquid chromatography (HPLC) is a powerful tool for the enantioselective separation of chiral drugs. However, the selection of an appropriate chiral stationary phase (CSP) and suitable operating conditions is a bottleneck in method development and a time- and resource-consuming task. Multimodal screening of a small number of CSPs with broad enantiorecognition abilities has been recognized as the best strategy to achieve rapid and reliable separations of chiral compounds. This paper describes the generic screening strategy developed at Johnson & Johnson Pharmaceutical Research and Development (J&J PRD) to successfully develop enantioselective HPLC methods for chiral molecules of pharmaceutical interest.
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Improved LC–MS Performance — A Three-Step Method for Minimizing Background Signals and Increasing Ionization EfficiencyOne problem frequently encountered in LC–MS is the appearance of mass peaks, which appear totally unrelated to the samples run - "ghost" mass peaks. It is impossible to differentiate whether these signals come from an unknown component in the sample co-eluting with a known peak, or from an impurity in the mobile phase or from some residual contamination "bleeding" from the column.
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Analysis of Secondary Metabolites from Myxobacteria using ESI-TOF–MS and PCAThe exploration of myxobacterial metabolite profiles by LC–MS screening for the presence of new natural products is described. Extracts from fermentations of Myxococcus strains are analysed by UPLC-coupled ESI-TOF mass spectrometry and the obtained data are processed using principal component analysis (PCA). The generation of molecular formulae from accurate mass measurements facilitates rapid compound identification.
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IC–ICP–MS for Monitoring the Fate of Iodinated X-ray Contrast Media after OzonationThis article shows the potential of IC–ICP–MS for monitoring iodine-containing ionic oxidation by-products that form during ozonation of iodinated X-ray contrast media.
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Instrument Considerations in the Transfer of Chromatographic Methods, Part III: Aligning Performance of ModulesIn method transfer, carefully aligning the modules of the two systems is essential.
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Automated Off-Line Two-Dimensional LC–MS–MS of Complex Proteomic Samples with the UltiMate 3000 SystemMultidimensional liquid chromatography (MDLC) techniques are essential for the separation of highly complex proteomic samples. Advantages of off-line MDLC techniques over on-line approaches include high flexibility in choice of column dimensions and mobile-phase compositions, and the ability to reanalyse sample fractions. Here we present a fully automated off-line two-dimensional chromatographic approach for the analysis of proteomic samples using an UltiMate 3000 system optimized for proteomics MDLC.
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Advancements in Tissue Lipidomics Hold Promise for Understanding Cardiovascular HealthIn a recent review article, researchers from Concordia University examined recent advancements in LC–MS workflows for tissue lipidomics.
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Quality Control and Advanced Characterization of MembranesBecause GPC is a reliable, simple and fast characterization method it can be readily adopted to investigate the separation behaviour of membranes.
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Electron-Capture Dissociation in a Radio-Frequency Linear Ion TrapHere we describe a new compact device for electron-capture dissociation (ECD) analysis of large peptides and posttranslational modifications of proteins, which can be difficult to analyze via conventional dissociation techniques such as collision-induced dissociation (CID). The new compact device realizes ECD in a radio frequency (RF) linear ion trap equipped with a small permanent magnet, which is significantly different than the large and maintenance-intensive superconducting magnet required for conventional ECD in Fourier-transform ion cyclotron resonance mass spectrometers. In addition to its compactness and ease of operation, an additional merit of an RF linear ion trap ECD is that its reaction speed is fast, comparable to CID, enabling data acquisition on the liquid-chromatography (LC) time scale. We interfaced the linear-trap ECD device to a time-of-flight mass spectrometer to obtain ECD spectra of phosphorylated peptides injected into a liquid chromatograph, infused glycopeptides, and intact small..
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Coupling Columns and Multidimensional Configurations to Increase Peak Capacity in Liquid ChromatographyAn overview is presented of possible pathways to enhance peak capacity in liquid chromatography (LC). The peak capacity in a chromatographic separation is directly related to the plate number and thus to column length and particle size. Serial coupled columns can be used to obtain long effective column lengths, reaching over 100000 theoretical plates and peak capacities up to 900. Some theoretical considerations are made on column dimensions and particle size and examples are given of high resolution "GC-like" separations in LC using state-of-the-art LC hardware. Recent developments in LC hardware have also enhanced the applicability of two-dimensional LC–LC and comprehensive LCÃ-LC. Both techniques are extremely powerful to unravel complex samples.
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Electron-Capture Dissociation in a Radio-Frequency Linear Ion TrapHere we describe a new compact device for electron-capture dissociation (ECD) analysis of large peptides and posttranslational modifications of proteins, which can be difficult to analyze via conventional dissociation techniques such as collision-induced dissociation (CID). The new compact device realizes ECD in a radio frequency (RF) linear ion trap equipped with a small permanent magnet, which is significantly different than the large and maintenance-intensive superconducting magnet required for conventional ECD in Fourier-transform ion cyclotron resonance mass spectrometers. In addition to its compactness and ease of operation, an additional merit of an RF linear ion trap ECD is that its reaction speed is fast, comparable to CID, enabling data acquisition on the liquid-chromatography (LC) time scale. We interfaced the linear-trap ECD device to a time-of-flight mass spectrometer to obtain ECD spectra of phosphorylated peptides injected into a liquid chromatograph, infused glycopeptides, and intact small..
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A New Tool for Mass Analysis of Unknown Molecules: High-Resolution Multistep Tandem MS with Wide Dynamic Range Quantitative AnalysisMass spectrometers are effective for identifying and quantifying unknown molecules, such as disease-related proteins and small molecules in pharmaceutical research and medical diagnosis. In addition, mass spectrometry (MS) can be particularly powerful when analyzing molecules with complex structures, such as posttranslationally modified proteins. Among various MS approaches, high-resolution multistep tandem MS (MS-MS) is an emerging methodology for accurate identification of complex molecules. In this article, we describe a new approach for mass analysis with enhanced quantitative capability combined with high-resolution multistep MS-MS, where the dynamic range of quantitation covers four orders of magnitude.
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Planar Chromatography Versus Column Chromatography: A Performance ComparisonIt is hypothesized that in particular cases, conventional planar chromatography provides a more effective and robust system than column chromatography with regard to separation efficiency and peak distribution of mixtures composed of low-retarded analytes. Under similar reversed-phase experimental conditions, a regular distribution of thin-layer chromatography (TLC) spots of four natural estrogens (estetrol, estriol, 17?-estradiol, and estrone) corresponds to strong irregular dispersion of peaks in chromatograms generated by high performance liquid chromatography. In both cases, the efficiency of separation was assessed using simple optimization criteria such as selectivity (?min) and resolution (Rs min). The distribution of chromatographic spots was evaluated using the relative resolution product (r). The results revealed that an excellent separation of the components of interest could be achieved easily using simple nonforced and isocratic TLC. Such an interesting property of planar chromatography is mainly driven by the nonlinear relationship between k and Rf retention factors. This article also reports the practical advantages of TLC for the separation of estrogenic steroid mixtures at different temperatures.
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Facilitated Column Selection in Reversed-Phase Liquid Chromatography for Pharmaceutical SeparationsThis article gives an overview of the performance of a previously developed system for the ranking of C18 reversed-phase columns applied to different pharmaceutical analyses. The separation of eight different drug substances from their respective impurities was studied. The chromatographic procedure for acetylsalicylic acid, clindamycin hydrochloride, buflomedil hydrochloride, chloramphenicol sodium succinate, phenoxymethylpenicillin and nimesulide was performed according to the corresponding European Pharmacopoeia monograph. The separations of dihydrostreptomycin sulphate and vancomycin were performed according to literature. It was found that that the column ranking system is a helpful tool in the selection of suitable columns in these analyses.
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High-Throughput Quantitative LC-MS-MS Assays by On-Line Extraction Using Monolithic SupportLC-MS-MS has become a widely used technique for the fast and sensitive quantitation of small molecules. In this article, this approach has been extended to high-throughput quantitative LC-MS-MS analysis under GLP applications for a drug candidate in development from preclinical animal studies through clinical development.
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A New Tool for Mass Analysis of Unknown Molecules: High-Resolution Multistep Tandem MS with Wide Dynamic Range Quantitative AnalysisMass spectrometers are effective for identifying and quantifying unknown molecules, such as disease-related proteins and small molecules in pharmaceutical research and medical diagnosis. In addition, mass spectrometry (MS) can be particularly powerful when analyzing molecules with complex structures, such as posttranslationally modified proteins. Among various MS approaches, high-resolution multistep tandem MS (MS-MS) is an emerging methodology for accurate identification of complex molecules. In this article, we describe a new approach for mass analysis with enhanced quantitative capability combined with high-resolution multistep MS-MS, where the dynamic range of quantitation covers four orders of magnitude.
Latest:
Electron-Capture Dissociation in a Radio-Frequency Linear Ion TrapHere we describe a new compact device for electron-capture dissociation (ECD) analysis of large peptides and posttranslational modifications of proteins, which can be difficult to analyze via conventional dissociation techniques such as collision-induced dissociation (CID). The new compact device realizes ECD in a radio frequency (RF) linear ion trap equipped with a small permanent magnet, which is significantly different than the large and maintenance-intensive superconducting magnet required for conventional ECD in Fourier-transform ion cyclotron resonance mass spectrometers. In addition to its compactness and ease of operation, an additional merit of an RF linear ion trap ECD is that its reaction speed is fast, comparable to CID, enabling data acquisition on the liquid-chromatography (LC) time scale. We interfaced the linear-trap ECD device to a time-of-flight mass spectrometer to obtain ECD spectra of phosphorylated peptides injected into a liquid chromatograph, infused glycopeptides, and intact small..
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Recent Advances in Bioanalytical Mass Spectrometry and Their Application to Marine ToxinsAn overview of some recently developed mass spectrometry techniques and their applications to marine biotoxins.
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Seamless Method Transfer from UPLC Technology to Preparative LCUltraPerformance LC (UPLC) has been widely accepted by chromatographers because of improvements over HPLC in the sensitivity, resolution and speed of separations. As scientists begin to use this technology for impurity and metabolite profiling, they will need to transfer the methods to preparative LC to isolate and purify their compounds for further research. Therefore, it is necessary to systematically transfer UPLC assays not only to HPLC, but, more importantly, to preparative chromatography. In this application, we provide information on how to scale a UPLC impurity/degradant separation to a preparative LC separation.
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Thermal Desorption-GC–MS Analysis of Polycyclic Aromatic Hydrocarbons on Fine Particulates in AirPolycyclic aromatic hydrocarbons (PAHs) are commonly found throughout the environment in soil, water and adsorbed to fine particulate matter in air. Of the 16 common PAHs, 7 have been classified as animal carcinogens by the International Agency for Research on Cancer (IARC). Resulting from this classification, PAHs are monitored and regulated in the environment.
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Fast Analysis of Malt Whisky by GC–MS Using an Ultra High Performance VF-WAXms Column from Varian, Inc.The flavours of malt whisky result from a complex blend of long chain esters and alcohols, derived from the distillation products and the composition of the wooden barrels in which the finished product is aged. As shown below, the new VF-WAXms column from Varian, Inc. is ideal for analysing whisky, especially when trace analysis is needed. The column's ultra-low bleed increases sensitivity, extends column life and improves accuracy, even at higher temperatures. In addition, VF-WAXms columns are suitable for use with MS detectors, as the ultra low bleed eliminates interferences and permits more sensitive detection.
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Different Approaches to Synthesizing Molecularly Imprinted Polymers for Solid-Phase ExtractionMolecularly imprinted polymers (MIPs) are synthetic polymeric materials that mimic immunosorbents. They are widely used as sorbents for solid-phase extraction (SPE). The most common way to synthesize them is bulk polymerization because of its simplicity and versatility. This produces a hard monolith that has to be ground and sieved to obtain particles in the desired size range. However, the partial loss of the materials as fine dusts; the irregular shape of the particles produced and their wide size distribution, have led to a search for different polymerization methods to offset the drawbacks of the bulk polymerization process.
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Automated High-Throughput Formula Determination and Confirmation with "sub-ppm" ConfidenceCombining an ultra fast LC system (e.g., Agilent 1200RRLC, Waters UPLC) with an accurate mass TOF mass spectrometer creates a powerful system for information-rich high-throughput analyses. However, for de novo formula generation and confirmation the residual mass accuracy tolerance of 3–5 ppm can still leave significant ambiguity in the proposed formula. Consequently, skilled manual inspection or further measurements deploying additional analytical techniques (NMR or MS–MS) are frequently required to arrive at a confident formula assignment.
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Leading Light: Pavel JanderaPavel Jandera spoke to Frantisek Foret about building his own liquid chromatograph, the birth of “modern” high performance liquid chromatography (HPLC), the importance of exploring (and understanding) earlier research papers, current trends in contemporary chromatography, and his inspiring advice for aspiring chromatographers.
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A New Tool for Mass Analysis of Unknown Molecules: High-Resolution Multistep Tandem MS with Wide Dynamic Range Quantitative AnalysisMass spectrometers are effective for identifying and quantifying unknown molecules, such as disease-related proteins and small molecules in pharmaceutical research and medical diagnosis. In addition, mass spectrometry (MS) can be particularly powerful when analyzing molecules with complex structures, such as posttranslationally modified proteins. Among various MS approaches, high-resolution multistep tandem MS (MS-MS) is an emerging methodology for accurate identification of complex molecules. In this article, we describe a new approach for mass analysis with enhanced quantitative capability combined with high-resolution multistep MS-MS, where the dynamic range of quantitation covers four orders of magnitude.
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Solid-Phase Extraction pipette Tip Sample Preparation for Membrane Protein Intact Mass Analysis by MALDI–MSAnalysis by mass spectrometry (MS) of integral membrane proteins and those associated with membrane is an important aspect of proteomics.
