LCGC Europe-05-01-2007

Over the years, LC instrumentation has undergone continuous development in pursuit of greater performance. More recently, the focus of progress has been on shorter run times, as a direct response to greater user demand to perform faster chromatographic analyses, particularly for their LC–MS applications. This has led to separations on short (30–50 mm) columns with a small internal diameter (i.d. ~2.0 mm), packed with small particle size phases (1.5–3.0 μm). The trend for smaller column particle size has now reached a practical limit on current hardware and innovative technological solutions for further gains in performance are required. Several manufacturers offer fast LC instruments designed for greater productivity, while maintaining low carryover, high sample capacity, resolution and reliability. With ultra-fast run times of under 1 minute, these companies have achieved increased throughput using contrasting technological approaches. Here we examine the background to this current trend,..

Although the majority of solid-phase extraction (SPE) is performed with conventional bonded silica- and polymeric-phases, difficult and complex samples may require more specialized stationary phases. In this instalment of "Sample Preparation Perspectives", columnist Ron Majors discusses advanced topics such as multimodal SPE, restricted-access media, molecular imprinted polymers, immunoaffinity extraction phases and other class-or compound-specific sorbents. These phases provide additional selectivity and procedures using them can be automated. Representative applications will be presented.

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This article describes the development of a routine method to analyse epoxidized soybean oil (ESBO) in baby food based on a previous method devised by Castle et al. The aim was to simplify the work-up procedure to reduce the strain on the analytical equipment. The extraction procedure was miniaturized to improve handling, reduce the resources needed and simplify the method. After derivatization, the extracts were cleaned using gel permeation chromatography (GPC). A modified gas chromatography mass spectrometry (GC–MS) method using pulsed splitless injection was developed to determine the analyte. For quality control (QC), peak area ratios (PARs) were calculated and evaluated in terms of functionality under routine conditions. The method was validated according to EU regulations at a level of 20 ppm and showed high reproducibility. The miniaturized method proved to be applicable to all investigated baby food matrices and demonstrated the benefits of a GPC clean-up step to reduce strain on the..

...it is important to acknowledge that environmental concerns can be more important than the economics of the reduction of solvent consumption.