Chromatography & Mass Spectrometry

A selection of articles from European Pharmaceutical Review covering Chromatography and Mass Spectrometry:


Universal detection in high performance liquid chromatography

Universal detection in high performance liquid chromatography

3 July 2015  •  David P. Elder, Phil Borman and George Okafo - GlaxoSmithKline

The most commonly used analytical technique for the testing of drug molecules is reversed-phase high performance liquid chromatography (RP-HPLC) with ultraviolet (UV)/visible detection. However, one of the biggest constraints affecting UV/visible detectors is their inability to generate adequate sensitivity for analytes lacking a suitable UV chromophore. These compounds comprise a surprisingly large group, encompassing natural products, particularly fermentation products, carbohydrates, lipids, certain amino acids, steroids, bisphosphonates, alkylating agents, excipients, polymer, surfactants, etc. (see Figure 1, page 50, for some representative structures). Secondly, it is often assumed that response factors for impurities are the same as for the parent when using UV detection systems, when often they are not. Accordingly, purity assessments are inevitably compromised to some degree. This short review will look at the use of some newer detection systems and the pros and cons of the various detector types. Hyphenated techniques such as HPLC-NMR and HPLC-MS have been deliberately excluded...

LC-MS Supplement

LC-MS: In-depth focus 2015

20 April 2015  •  David Elder, Phil Borman, George Okafo, William McDowell, Hanne Røberg-Larsen

In this free-to-view LC-MS in-depth focus, we delve into the world of glycans, and how their natural complexity necessitates sophisticated sequencing techniques, while another article aims to demonstrate the versatility of LC-MS and the ease with which it can be combined with a variety of MS systems, focusing particularly on nanoLC...

HPLC: On-chip liquid chromatographic separation

HPLC: On-chip liquid chromatographic separation

17 April 2015  •  Makoto Tsunoda, University of Tokyo

High-performance liquid chromatography (HPLC) is a powerful separation technique due to its high accuracy, precision, versatility and robustness. In the development of pharmaceuticals, it is no doubt that LC is a key technology in the quality control of pharmaceuticals and pharmacokinetic studies and in the analysis of complex biological compounds in bio-samples for the clarification of the function of biological systems. Nowadays, pharmaceutical developments require that HPLC analyses are fast and efficient. However, reducing separation times in LC without reducing the separation efficiency requires generating higher resolving power per unit time while speeding separation times without lessening the quality of the separation enables important analytical information to be generated more quickly. To achieve these goals in LC, monolithic column, high-temperature LC, fused-core column and ultra high-pressure LC with sub-2µm particles packed into column have been developed. This review will focus on chip-based pressure-driven LC separation...

David Elder

Can HPLC assay methods really be considered quality critical tests?

5 September 2014  •  Dave Elder, GlaxoSmithKline and JPAG

Analytical method specificity is assessed using ICH (International Conference on Harmonisation) Q2 (2005). Although, certain methods are not specific enough for their intended purposes, they may have other advantages. Both titrimetric and UV (Ultra-violet spectroscopy) assays are non-specific, but have superior precision (ca. 0.1-0.5% RSD (Residual Standard Deviation)) compared with the corresponding specific HPLC (High Performance Liquid Chromatography) assay methods (>0.5% RSD)...

Mass spectrometry-based metabolics – an exclusive online-only article from Tun-Li Shen at Brown University

3 July 2014  •  Tun-Li Shen, Brown University

Tun-Li Shen provides a brief overview of the gas chromatography mass spectrometry (GC-MS) and liquid chromatography mass spectrometry (LC-MS) instrumentation platforms used in untargeted metabolomics studies...

Mass Spectrometry In-depth focus

Mass Spectrometry: In-depth focus 2014

15 April 2014  •  Paul J. Gates, Ioannis Papayannopoulos

In this free-to-view in-depth focus: Some tricks and tools for structural characterisation of natural products using Electrospray mass spectrometry, Mass spectrometry in the biopharmaceutical industry: from the mundane to the cutting edge, and Mass Spectrometry roundtable...

Birthe V. Nielsen, Faculty of Engineering and Science, University of Greenwich

Practical considerations in analysing biologically active peptides by Electrospray Ionisation (ESI) Mass Spectrometry

22 October 2013  •  Birthe V. Nielsen, Faculty of Engineering and Science, University of Greenwich

Neuromodulators such as calcitonin gene-related peptide (CGRP) and vasoactive intestinal peptide (VIP) act as biomarkers for pain assessment (pre-clinical). These markers can be detected at low concentrations by Electrospray Ionisation (ESI) Mass Spectrometry (MS). Currently, little is known about the factors affecting responsiveness in the ESI process though the response of peptide ions depends heavily on analyte basicity in solution, pKb, sampling and instrumental conditions. Other factors may be equally important, however, not enough is known about the link between peptide characteristics and selectivity in the ESI process. Here, we review our findings on these links to improve the analyte signal and allow robust quantitation of these important peptide biomarkers...

Mass Spectrometry Supplement 2013

Mass Spectrometry: In-depth focus 2013

17 April 2013  •  Uwe Christians, Jelena Klawitter, Jost Klawitter, George McLeod, Min Yang

Corticosteroids and mass spectrometry; latest applications using LC/MS3.
Multi-analyte LC-MS/MS assays for the quantification of endogenous compounds during the development of drugs and companion diagnostics...

Figure 1: Sample preparation techniques for mass spectrometry based pharmaceutical and metabolite analysis. The three approaches discussed in the paper are outlined: (Top) mass spectrometry imaging from dosed tissue sections, (Middle) liquid chromatography mass spectrometry of tissue extracts or plasma/serum samples, (Bottom) gas chromatography mass spectrometry of plasma/serum samples

MS-based methods for detection, quantitation and localisation of pharmaceuticals and metabolites in biological samples

18 December 2012  •  Tyler Greer, Department of Chemistry, University of Wisconsin-Madison and Lingjun Li, Department of Chemistry & School of Pharmacy, University of Wisconsin-Madison

Mass spectrometry is a powerful, multi-faceted technique capable of analysing pharmaceuticals and their metabolites in biological matrices. Although it is more commonly applied to proteins, peptides and lipids, an increasing number of studies use mass spectrometry based techniques to detect, quantitate and localise pharmaceuticals and their metabolites. The availability of functionally unique ionisation methods and preparative separation options coupled with the specificity and sensitivity of a mass analyser make mass spectrometry an attractive option in pharmaceutical studies involving biofluids and tissue. This review aims to provide a general description of the primary mass spectrometric and preparative steps used to analyse pharmaceuticals in biological systems...

In-Depth Focus: Mass Spectrometry

In-depth focus – Mass Spectrometry

25 April 2012  •  Ana Rita Angelino, Min Yang, Tasso Miliotis, Constanze Hilgendorf, Anthony Bristow, George McLeod, Detlev Hochmuth, Alessandro Baldi, Gary Harland

Mass spectrometry in drug discovery - Proteomics, small molecules and metablomics.
Quantification of membrane drug transporters and application in drug discovery and development.
Mass spectrometry leaders roundtable.

Recent developments in the use of LCMS in process pharmaceutical chemistry

28 February 2012  •  Dr. Florence O. McCarthy, Department of Chemistry, Analytical and Biological Chemistry Research Facility, University College Cork

Liquid Chromatography Mass Spectrometry (LCMS) is a powerful technique that has recently undergone exponential growth in its application to pharmaceutical synthesis. This perspective will outline the general principles of LCMS, detail some recent approaches and the benefits to be derived from its use at an early stage of process development. Identification of the components in a mixture is the primary function of analytical chemistry and there are a range of techniques available. When the solution to this problem requires some structural identity, LCMS is the instrument of choice. Liquid Chromatography Mass Spectrometry is defined as the use of the separating properties of liquid chromatography combined with a detector capable of mass analysis (mass spectrometer: single quadrupole, triple quadrupole, ion trap, Time Of Flight, Q-TOF etc.). This combination may be configured in many ways, for a general scheme...

FIGURE 1 Schematic overview of the MALDI-MSI process as applied to imaging compound and metabolite distributions in a whole body rat sample. From one section of an animal dosed with the unlabelled compound, the substance and metabolite distributions can be acquired

MALDI-mass spectrometry imaging applied to drug discovery and development

19 October 2011  •  Brendan Prideaux, Dieter Staab, Gregory Morandi, Nicole Ehrhard and Markus Stoeckli, Novartis Institutes for BioMedical Research

Since its introduction in the field of biomedical imaging over 10 years ago, matrixassisted laser desorption/ionisation mass spectrometry imaging (MALDI-MSI) has played an ever increasing role in drug discovery and development and is now utilised in laboratories of many leading pharmaceutical companies and collaborating academic institutions. The need for mass spectrometry imaging in drug discovery is founded on the shortcomings of current technologies. Traditional methods of spatially mapping the distribution of compounds in tissue involved a combination approach of autoradiography (WBA) with metabolite information obtained from LC/MS analysis of tissue homogenate. Autoradiography methods only monitor the radiolabel and therefore are not able to distinguish the parent drug from its metabolites. The addition of LC/MS allows for conclusive determination of metabolites. However, this only produces spatial information at the whole organ level and not the spatial detail that can be routinely achieved using MSI...

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