LCGC Europe-08-01-2016

The 33rd International Symposium on Microscale Separations and Bioanalysis (MSB 2017) will be held from 26–29 March 2017, at Conference Center de Leeuwenhorst, The Netherlands, in the “largest flower garden of Europe” near to Amsterdam International Airport and North Sea beaches.

Systematic toxicological analysis (STA) is an important step in medicolegal investigations of death, poisoning, and drug use. The primary goal is the detection and confirmation of potentially toxic compounds in evidence. This article describes a workflow using non-targeted liquid chromatography–tandem mass spectrometry (LC–MS/MS) for reliable compound identification. Tandem mass spectrometry was performed on a low-resolution quadrupole-quadrupole-linear ion trap instrument. Acquired spectra were submitted to automated library search, and positive matches were verified by expert reviewing. After validation, the non-targeted LC–MS/MS technique was integrated in the STA service provided by our laboratory.

Adequate detection of trans-resveratrol in wine is complicated by two factors: relatively low levels and interferences from matrix components. Here, we present two useful approaches to overcoming these issues depending on the instrumentation available. For high performance liquid chromatography (HPLC) analyses with ultraviolet (UV) detection, matrix peaks can be removed by microextraction using a packed sorbent while simultaneously concentrating the trans-resveratrol peak by a factor of two. For liquid chromatography–mass spectrometry (LC–MS), the extracted ion chromatogram for the [M + H]+ analyte ion can be used to obtain specificity without prior extraction procedures.

Detectors based on ultraviolet absorbance are the most common detectors in use for liquid chromatography.

The past couple instalments of “Sample Preparation Perspectives” have looked at current trends in the field. Another recent trend is dried blood spot analysis and other analysis methods using minute sample amounts. This month we take a quick look at the role of sample homogeneity and the determination of sample size. Microsampling approaches, including dried blood spots, are discussed.

This fourth and last instalment in the “Separation Science in Drug Development” series provides an overview of modern practices of quality control in small-molecule drug development, including activities such as setting specifications, method validation and transfer, release and stability testing, and authoring chemistry, manufacturing, and controls (CMC) sections of regulatory filings.

A selection of profiles on leading separation science companies.

Click the title above to open the LCGC Europe August 2016 regular issue, Vol 29, No 8, in an interactive PDF format.

Supplementary Tables