Special Issues-10-03-2016

An introduction from the guest editors of this special supplement from LCGC Europe revealing recent developments in small-molecule drug analysis.

Sample preparation techniques in bioanalysis are multistep, time-consuming, and labour-intensive procedures that can take up 60–80% of the total analysis time. Sample preparation is often the limiting step of fast bioanalysis and the most error-prone part of the analytical method. There is currently a focus on improving the sample preparation process by shortening sample preparation time, cutting the cost of analysis, decreasing sample volume and solvent consumption, reducing the number of sample preparation steps, and adapting the whole process for automation. This article explores microextraction techniques, selective approaches, on-line sample preparation, and dried matrix spots that aim to provide solutions to sample preparation problems in bioanalysis.

Quality by design (QbD) has gained in importance in the pharmaceutical industry and is supported by several regulatory documents (ICH, FDA). The aim is to ensure product quality through a better understanding of products and processes during pharmaceutical development. As analytical procedures are critical processes of pharmaceutical product development and quality control (QC), QbD has become a key tool in the development of analytical methods. This article outlines the general trends observed when applying QbD to the development of separation methods in pharmaceutical analysis. The main pharmaceutical applications are reviewed along with a detailed description of tools involved in QbD methodology. A focus on QbD benefits for the pharmaceutical industry is provided.

The new generation of high-resolution mass spectrometry (HRMS) systems offers high sensitivity, dynamic range, resolution, accuracy, and scan-to-scan reproducibility, enabling high-throughput quantitative analyses in combination with information-rich qualitative data. The most recently released HRMS systems offer an alternative to triple quadrupole (TQ)-MS systems. This provides a huge opportunity to obtain quantitative and qualitative information from one analysis, but also requires a different mindset and expertise to make the right choices and compromises to get the most information from your sample.

The first high performance liquid chromatography (HPLC) column for enantioselective chromatography was introduced commercially in 1981. This chromatographic mode has now become the method of choice for the analysis of chiral pharmaceutical compounds, making previous approaches, such as optical rotation, almost completely obsolete. However, supercritical fluid chromatography (SFC) has been gaining increasing recognition as a complementary technique to HPLC for pharmaceutical enantioselective analysis. Gas chromatography (GC) and capillary electrophoresis (CE) remain very useful for particular applications.

The proportion of counterfeit medicines has increased dramatically. Combatting this issue is complex, and various levels of action are necessary. The quality control (QC) of imported batches using simple, reliable, and cost-efficient analytical approaches is vital. Capillary electrophoresis (CE) is becoming important because the analysis is achieved in a capillary with small dimensions, and is usually filled with an aqueous buffer. No organic solvent is required and injection volumes are in the nanolitre range, which is convenient because of the low availability of reference substances and reduces the environmental impact. CE is now recognized by numerous Pharmacopeia and can be used for counterfeit and substandard characterization as a validated analytical procedure that adheres to international guidelines.

Click the title above to open the LCGC Europe October 2016 Advances in Pharmaceutical Analysis Supplement, Vol 29, No s10, in an interactive PDF format.