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A summary of the most recent advances in sample preparation, instrumentation, and data-processing techniques for MALDI-IMS

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This instalment of Tips & Tricks focuses on whether a complete separation can be achieved using GPC/SEC and, if so, under what conditions.

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This installment provides an overview of high-throughput characterization techniques of drug leads to support small molecule drug discovery programs in a pharmaceutical company. A myriad of analytical chemistry techniques including separation science methodologies are used to confirm the structures and identities, quantitating the concentrations of stock solutions, and measuring key physicochemical properties of the new chemical entities (NCE). A case study is used here to illustrate the details of these applications in high-throughput characterization.

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Here in part II of our series on assessing protein aggregation, we provide an overview of best practices for achieving this goal, including the importance of using a multimethod approach.Here in part II of our series on assessing protein aggregation, we provide an overview of best practices for achieving this goal, including the importance of using a multimethod approach.

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To measure a method’s environmental friendliness and its sustainability, one must consider its productivity and analytical performance.

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A summary of the most recent advances in sample preparation, instrumentation, and data-processing techniques for MALDI-IMS

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A CHIRALPAK IG column (immobilized meta selector) was used to develop the enantioselective separation of methylclothiazide. Meta-substituted immobilized chiral selectors have been shown to have remarkable affinity for resolution of chiral compounds from different types of molecules.

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This application note presents a gradient method using a core–shell column for the determination of various substances in Bourbon vanilla extracts as well as in natural and artificial vanilla flavours. The aim is to compare the ingredients to achieve proof of the authenticity of Bourbon vanilla. By applying the Knauer AZURA Analytical system, a very short analysis time and low eluent consumption could be achieved. The high speed and reliability of the method makes it well-suited for routine analyses in food control.

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Ion-mobility spectrometry (IMS) is an anlytical technique that provides for the separation of ions in the gas phase. The separation, occuring on a timescale of milliseconds, is based on the differing mobility of ions according to their charge, shape, and size. These characteristics make IMS suitable for coupling with mass spectrometry (MS), to serve in current MS-based workflows for metabolomics and lipidomics. IM-MS improves peak capacity and signal-to-noise ratios, and it provides more confidence during compound identification or confirmation than conventional analyses. Combining collision-induced dissociation with ion-mobility separation improves the specificity of MS/MS-based approaches. Significantly, ion-mobility-derived information provides an orthogonal, physicochemical parameter-the collision cross section (CCS)-which relates to a metabolite's shape. Novel hardware and software solutions enable analysts to process and exploit IMS-MS data for qualitative and quantitative metabolomics and lipidomics applications.

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A simple and accurate method for determining trace level of carcinogenic solvent carbon tetra chloride (CCl4) in Flunixin Meglumine, a drug substance which is white crystalline powder was developed by Gas chromatography .The method was observed to be robust and complete analytical method validation was performed and meets the requirements as per ICH guidelines. The method possesses the lowest detection level when compared with other methods currently available. The LOQ achieved by this method was 0.8 ppm and calibration curves were linear, R >0.998.In general, for analysis of halogenated compounds electron capture detector (ECD) were mostly used and in this proposed method flame ionization detector (FID) with internal standard was used. The method was implemented for various Active pharmaceutical ingredients (API) successfully.

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A simple and accurate method for determining trace level of carcinogenic solvent carbon tetra chloride (CCl4) in Flunixin Meglumine, a drug substance which is white crystalline powder was developed by Gas chromatography .The method was observed to be robust and complete analytical method validation was performed and meets the requirements as per ICH guidelines. The method possesses the lowest detection level when compared with other methods currently available. The LOQ achieved by this method was 0.8 ppm and calibration curves were linear, R >0.998.In general, for analysis of halogenated compounds electron capture detector (ECD) were mostly used and in this proposed method flame ionization detector (FID) with internal standard was used. The method was implemented for various Active pharmaceutical ingredients (API) successfully.

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Ionic liquids (ILs) have become recognized in gas chromatography (GC) as stable and highly polar stationary phases with a wide application range. Having customizable molecular structures, ILs also offer a particular tunability that provides additional selectivity, and therefore may improve separation for neighbouring analytes. This article presents specific properties of IL phase capillary GC columns, including polarity scale and inner surface morphologies of IL columns. Application of IL phases in achiral and chiral GC, and multidimensional GC, are highlighted.

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Ionic liquids (ILs) have become recognized in gas chromatography (GC) as stable and highly polar stationary phases with a wide application range. Having customizable molecular structures, ILs also offer a particular tunability that provides additional selectivity, and therefore may improve separation for neighbouring analytes. This article presents specific properties of IL phase capillary GC columns, including polarity scale and inner surface morphologies of IL columns. Application of IL phases in achiral and chiral GC, and multidimensional GC, are highlighted.

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Ionic liquids (ILs) have become recognized in gas chromatography (GC) as stable and highly polar stationary phases with a wide application range. Having customizable molecular structures, ILs also offer a particular tunability that provides additional selectivity, and therefore may improve separation for neighbouring analytes. This article presents specific properties of IL phase capillary GC columns, including polarity scale and inner surface morphologies of IL columns. Application of IL phases in achiral and chiral GC, and multidimensional GC, are highlighted.

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A team of chemists and microbiologists from the University of Leicester has developed a new method of rapidly diagnosing the infection Clostridium difficile (C. difficile).

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Resistive glass tubes and plates are designed to guide ions by generating a uniform electric field. Photonis resistive glass products are composed of a proprietary lead silicate glass that has been specially processed to create a resistive layer at the surface. The resistivity can be varied over several orders of magnitude to suit the specific application.

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This 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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This 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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The lack of proper method validation has important implications in blood alcohol concentration (BAC) determinations. We examine this issue, addressing the importance of gas chromatography (GC) for BAC determination, why certain validation procedures are important, and why accreditation bodies need to step up their game.

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The connection of a quantum spectral fingerprint to molecular structure makes spectroscopy ideal for chemical detection. Even with the broad utility of chromatography and mass spectrometry, there is still a rigor to expand the applicability of high resolution spectroscopy by miniaturizing FT-NMR and enhancing the performance of mid-IR techniques. While IR instrumentation experts have been incorporating the latest diode lasers, molecular rotational resonance (MRR) spectroscopists have designed a digital, solid-state approach to reach subTerahertz (millimeter/submillimeter-wave) molecular spectroscopy from the radio regime. Recent innovations for FT-MRR techniques have finally brought millimeter-wave spectroscopy into the modern age. FT-MRR spectroscopy is applied here to gas analyses, air analysis, and headspace analysis for sensitive, chemically specific detection of VOCs without the need for lasers, chemometrics, or chromatography.

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The connection of a quantum spectral fingerprint to molecular structure makes spectroscopy ideal for chemical detection. Even with the broad utility of chromatography and mass spectrometry, there is still a rigor to expand the applicability of high resolution spectroscopy by miniaturizing FT-NMR and enhancing the performance of mid-IR techniques. While IR instrumentation experts have been incorporating the latest diode lasers, molecular rotational resonance (MRR) spectroscopists have designed a digital, solid-state approach to reach subTerahertz (millimeter/submillimeter-wave) molecular spectroscopy from the radio regime. Recent innovations for FT-MRR techniques have finally brought millimeter-wave spectroscopy into the modern age. FT-MRR spectroscopy is applied here to gas analyses, air analysis, and headspace analysis for sensitive, chemically specific detection of VOCs without the need for lasers, chemometrics, or chromatography.

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The connection of a quantum spectral fingerprint to molecular structure makes spectroscopy ideal for chemical detection. Even with the broad utility of chromatography and mass spectrometry, there is still a rigor to expand the applicability of high resolution spectroscopy by miniaturizing FT-NMR and enhancing the performance of mid-IR techniques. While IR instrumentation experts have been incorporating the latest diode lasers, molecular rotational resonance (MRR) spectroscopists have designed a digital, solid-state approach to reach subTerahertz (millimeter/submillimeter-wave) molecular spectroscopy from the radio regime. Recent innovations for FT-MRR techniques have finally brought millimeter-wave spectroscopy into the modern age. FT-MRR spectroscopy is applied here to gas analyses, air analysis, and headspace analysis for sensitive, chemically specific detection of VOCs without the need for lasers, chemometrics, or chromatography.

Latest:

The connection of a quantum spectral fingerprint to molecular structure makes spectroscopy ideal for chemical detection. Even with the broad utility of chromatography and mass spectrometry, there is still a rigor to expand the applicability of high resolution spectroscopy by miniaturizing FT-NMR and enhancing the performance of mid-IR techniques. While IR instrumentation experts have been incorporating the latest diode lasers, molecular rotational resonance (MRR) spectroscopists have designed a digital, solid-state approach to reach subTerahertz (millimeter/submillimeter-wave) molecular spectroscopy from the radio regime. Recent innovations for FT-MRR techniques have finally brought millimeter-wave spectroscopy into the modern age. FT-MRR spectroscopy is applied here to gas analyses, air analysis, and headspace analysis for sensitive, chemically specific detection of VOCs without the need for lasers, chemometrics, or chromatography.

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Sample pre-treatment is one of the bottlenecks in analytical chemistry specially when dealing with complex matrices like environmental samples. When performed in a batch mode, sample handling methods are tedious and time consuming. Therefore, the hyphenation of these methods with flow injection techniques yields many advantages. The possibility of automation not only increases the determination rate, but also decreases sample and reagent consumption. As a consequence, analyte separation, enrichment, and elimination of sample matrix becomes possible with an increase in selectivity and sensitivity. This is a significant contribution for the analysis of environmental samples as the analyte is usually present at trace levels in a complex matrix. In this scenario, the state of the art of solid phase spectrometry (SPS) with a focus on the lab-on-valve (LOV) platform is discussed. LOV facilitates the manipulation of bead suspension for SPS with lower reagents consumption and waste production.