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Analysis by mass spectrometry (MS) of integral membrane proteins and those associated with membrane is an important aspect of proteomics.

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The structural complexity of monoclonal antibodies (mAbs) challenges the capabilities of even the most advanced chromatography and mass spectrometry techniques. This study examines the use of micro-pillar array columns in combination with mass spectrometry for peptide mapping of both mAbs and antibody–drug conjugates (ADCs).

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The International Symposium on the Separation and Characterization of Natural and Synthetic Macromolecules (SCM-X) will take place virtually, from 27 to 29 January 2021, with the live event potentially taking place in 2023. This preview offers a flavour of what visitors can look forward to from SCM-X’s “Zoomposium”.

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LC-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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The authors describe a sensible approach for validation and implementation of HPLC IPC assays.

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The 30-year history of advances in gas chromatography–mass spectrometry technology continues today. Recent improvements in hardware, electronics, and data analysis software have resulted in new levels of productivity and sensitivity that have broadened the potential applications for this laboratory mainstay.

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The results of a study to determine the influence of SEC column order on molecular size separation and peak broadening

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This 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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Protein and peptide analysis via tandem mass spectrometry (MS-MS) has resulted in a wealth of information regarding protein identification, structure, and abundance levels over the past 10 years. Techniques such as neutral loss scanning and collision-induced dissociation (CID) have been especially helpful in facilitating the identification of a multitude of previously unknown sites of protein phosphorylation. However, many of the techniques used to obtain this information are labor intensive and work inconsistently. To address this problem, much effort has been put forth to find alternative methods of fragmenting peptides and proteins that are less difficult and applicable to a wide gamut of peptide classes. Examples of recently developed dissociation techniques include infrared multiphoton dissociation (IRMPD) and electron transfer dissociation (ETD). The implementation of these new techniques has widened the spectrum of peptides amenable to tandem mass spectral analysis.

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Polynuclear aromatic hydrocarbons (PAHs) are carcinogenic condensed ring aromatic compounds widely found as trace pollutants in waters, wastes, air particulates, soil and foods. PAHs can be routinely monitored using HPLC with a combination of UV and fluorescence detection as prescribed in EPA methods 550.1, 610 and 8310.

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Over the years, LC instrumentation has undergone continuous development in pursuit of greater performance. More recently, the focus of progress has been on shorter run times, as a direct response to greater user demand to perform faster chromatographic analyses, particularly for their LC–MS applications. This has led to separations on short (30–50 mm) columns with a small internal diameter (i.d. ~2.0 mm), packed with small particle size phases (1.5–3.0 μm). The trend for smaller column particle size has now reached a practical limit on current hardware and innovative technological solutions for further gains in performance are required. Several manufacturers offer fast LC instruments designed for greater productivity, while maintaining low carryover, high sample capacity, resolution and reliability. With ultra-fast run times of under 1 minute, these companies have achieved increased throughput using contrasting technological approaches. Here we examine the background to this current trend,..

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Calvados is an apple-brandy of Normandy (France). Mashed apples are fermented to obtain cider and then distilled to give the young spirit.

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Since September 2008, 294,000 infants and young children suffered urinary problems due to the contamination of melamine in infant milk powder and were hospitalized. This hospitalization was required to treat the symptoms caused by the ingestion of melamine contaminated infant formula and related dairy products. Previously in 2007, pet food, animal feed, wheat gluten, and other protein-based foods were found to contain residues of melamine and its degradation product cyanuric acid (2).

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Combining 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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Presenting a novel chromatographic modelling method to establish QbD-compliant comparative testing of eluent design spaces.

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The separation of structurally diverse analytes is often complicated by chance coelutions with other analytes or with matrix related compounds. Often the column is blamed, but while such coelutions make analysis difficult they do not necessarily indicate a faulty column, poor chromatography or method design.

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It 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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his article reveals the first liquid chromatography (LC) separations performed on a microfabricated pillar array column under pressure-driven conditions. The pillars were non-porous and produced using a Bosch-type deep reactive ion etch (DRIE) to pattern the surface of a silicon wafer and had a diameter of approximately 5 μm. Two different packing densities were compared: one similar to the packing density of a packed bed (external porosity of approximately 49%) and one similar to the packing density of monolithic columns (external porosity of approximately 70%).

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The use of dual polarization interferometry (DPI) to measure the behaviour of alkyl-modified surfaces under different solvent regimes is described. The empirically observed and modelled behaviour of grafted long alkyl chain adlayers on a silica surface were in good agreement. The empirical data was also compared with data using analogous systems and these also matched well. This approach has the potential to gain much greater insight into the behaviour of reversed-phase (RP) columns and could help to design column surfaces that are resistant to phase collapse.

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In his article, published in 2000, David V. McCalley found large increases in the efficiency for basic compounds at elevated temperature

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Molecularly 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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This 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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Mass overload is related to the mass of sample that can be injected before the stationary phase is sufficiently loaded to cause changes in the chromatography.

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Protein/peptide discovery data obtained from data-dependent experiments have been used to increase the success rate of targeted quantification assays as well as automate method building.

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The use of dual polarization interferometry (DPI) to measure the behaviour of alkyl-modified surfaces under different solvent regimes is described. The empirically observed and modelled behaviour of grafted long alkyl chain adlayers on a silica surface were in good agreement. The empirical data was also compared with data using analogous systems and these also matched well. This approach has the potential to gain much greater insight into the behaviour of reversed-phase (RP) columns and could help to design column surfaces that are resistant to phase collapse.

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It makes intuitive sense - the higher the sensitivity of an inductively coupled plasma–mass spectrometry (ICP-MS) system, the lower the detection limit. But there are many factors that affect the detection limit for a given isotope in a given sample. These factors include sensitivity, background noise, and interferences.

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Switching the GPC/SEC solvent from THF to 2-methyl-THF provides an easy swap to provide a greener, safer, and less toxic option.

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The current status of superheated water extraction is reviewed, and the extraction methods, applications, and problems encountered are discussed.

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Everyone is talking about sustainability, and organizations are creating sustainability programs. But what does green chemistry really mean, and how does it apply to gas chromatography?