Recent Advances in Solid-Phase Microextraction, Part 1: New Tricks for an Old Dog
March 1st 2019Solid-phase microextraction (SPME) was introduced nearly 30 years ago and since that time has matured into a widely used tool in the arsenal of sample preparation techniques. Simultaneously, it has spawned a host of related techniques where sorbent coatings are placed on stir bars, magnetic particles, vial walls, and so on. Over the past few years, several advances in SPME have been developed, including increasing the sorbent surface area available for extraction, accommodating direct analysis by mass spectrometry (MS), and sorbent overcoating to resist fouling by sugars, lipids, and other macromolecules present in some sample types. These advances are discussed in this month’s instalment. The use of SPME for microsampling of biological systems, so-called bio-SPME, will be the focus of Part 2.
Perspectives on the Adoption and Utility of 1.0-mm Internal Diameter Liquid Chromatography Columns
March 1st 2019One millimetre internal diameter liquid chromatography columns are available from many manufacturers. In this article, the utility of 1.0-mm internal diameter (i.d.) columns, and the arenas in which they play a relatively strong role, are investigated. Further, the advantages and disadvantages of 1.0 mm diameter columns are contrasted with both larger- and smaller-bore formats.
Extraction of Loperamide and N-Desmethyl Loperamide from Blood Followed by LC–MS/MS Analysis
March 1st 2019This application note outlines a simple three-step method for the extraction of loperamide and its main metabolite, N-desmethyl loperamide, from blood. UCT’s Clean Screen® XCEL I column provides users with the same level of sample clean-up as traditional SPE while allowing the elimination of timely conditioning and wash steps.
Assessing Antibody ADCC Activity by Affinity HPLC
March 1st 2019Antibody-dependent cell-mediated cytotoxicity (ADCC) is a crucial mechanism of action (MoA) of anti-tumour therapeutic antibodies and FcγIIIa receptor plays a key role in this process by interacting with the N-glycans of IgG Fc regions. Hence, affinity chromatography on Fc receptor ligands can deliver valuable information about expected ADCC activity and mAb glycoform distribution.
Identifying Long-Chain and Short-Chain Branching in Polymers
March 1st 2019Branching affects macroscopic polymer properties such as crystallinity, melting temperature, toughness, ductility, and optical clarity. Two types of branching are long-chain branching (LCB) and short-chain branching (SCB), wherein the molar mass of the branches is larger or smaller than the entanglement molar mass, respectively.
Recent Advances in Comprehensive Chromatographic Analysis of Emerging Drugs
March 1st 2019This article discusses the use of emerging technologies that are complementary to established techniques, to significantly reduce these shortcomings for both synthetic cannabinoids and synthetic cathinones. In this vein, the utility of recently reported approaches including ultrahigh performance supercritical fluid chromatography (UHPSFC)–photodiode array (PDA) ultraviolet (UV)–MS, and GC–vacuum UV is discussed. To increase the specificity of analysis, multiple chromatographic techniques are commonly used. For the analysis of emerging drugs, a combination of GC and UHPSFC is recommended. The utility of a previously unreported coupled-columns approach for UHPSFC to significantly enhance resolution of synthetic cathinones is presented.
Drawing A Better Map: Recent Advances in Protein Digestion and Peptide Mapping
March 1st 2019Biotherapeutics have become the hottest topic in pharmaceutical research over the past decade. With the increased interest in biotherapeutics, there has been a concomitant increase in new analytical methods for characterizing these large, complex molecules. This installment of “Column Watch” discusses advances in “bottom-up” analysis of monoclonal antibodies, while highlighting the role and importance column chemistry still plays in developing highly selective high-performance liquid chromatography (HPLC) methods for peptides.
Plant Metabolomic Workflows Using Reversed-Phase LC and HILIC with ESI-TOF-MS
March 1st 2019In plant metabolomics, molecular fingerprints and additional molecular descriptors can be identified using recent developments in polarity-extended separations with serial coupling of reversed-phase LC and HILIC combined with ESI-TOF-MS.
The Benefits of Data-Independent Acquisition in Metabolomics
March 1st 2019Data-independent acquisition (DIA) makes it possible to re-interrogate data from earlier analyses to determine if new compounds have appeared in a sample previously analyzed. In this interview, Craig Wheelock of the Karolinska Institute discusses the use of DIA in metabolomics.