Special Issues-05-02-2013

This article highlights some selected examples of the power of liquid chromatography combined with mass spectrometry (LC–MS) in the development of protein biopharmaceuticals.

An introduction from the guest editors of this special supplement from LCGC Europe focusing on some recent developments in pharmaceutical analysis.

The determination of genotoxic impurities (GIs) in drug substances and pharmaceutical products is an emerging topic in pharmaceutical quality control. GIs are intermediates or reactants in the synthetic pathway of a drug substance and should be monitored at ppm (?g/g drug substance) or even ppb (ng/g) levels. This is several orders of magnitude lower than in classical impurity analysis (0.05% or 500 ppm level) or in residual solvent analysis. Analytical methods for the determination of GIs include gas chromatography (GC) and liquid chromatography (LC), both often combined with mass spectrometry (MS) detection. Some typical examples of GIs trace analysis using GC and LC are presented. The potential of on-line reaction monitoring is also discussed.

This article provides an overview of the most recent advances in the field of chiral and achiral separations in SFC. This involves research focused on the most critical parameters in SFC separations, but also on practical issues such as the serial coupling of columns.

Hydrophilic interaction liquid chromatography (HILIC) has recently become more important, particularly for the analysis of polar drugs, metabolites and biologically relevant compounds in glycomics, proteomics, metabolomics and clinical analysis. HILIC makes it possible to increase the retention of polar compounds, achieve orthogonal selectivity and increase mass spectrometry (MS) sensitivity, compared with reversed-phase liquid chromatography. This article discusses the advantages and limitations of HILIC in a variety of practical applications in the pharmaceutical industry.

A new technique was developed based on liquid chromatography coupled with tandem mass spectrometry to analyze drugs that are not part of current immunoassay screening, specifically zolpidem, zopiclone, and zaleplone, or "z-drugs." This method allows for the simultaneous quantification of the z-drugs and all major benzodiazepines in human urine samples.