Column: Sample Preparation Perspectives - LC-GC Europe
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Column: Sample Preparation Perspectives
  • Seeing Green


    Hian Kee Lee speaks with Alasdair Matheson about "environmentally friendly" sample preparation techniques.

    On-Site Sample Preparation Using MEPS for Wastewater Analysis


    Reports the qualitative field use of C18-MEPS for the sampling of water bodies in both industrial and urban environments.

    Immunosorbents for Selective Sample Preparation of Complex Mixtures


    Selective sample preparation techniques are particularly attractive for the analysis of trace amounts of small molecules in complex matrices. In this month's instalment, columnist Ron Majors covers the field of immunoextraction, a technique that employs immobilized antibodies to selectively capture specific analytes using molecular recognition via antibody–antigen interactions. Recently, the introduction of commercial products for specific high-volume environmental and food safety applications should spur further applications of this technique.

    QuEChERS — A New Technique for Multiresidue Analysis of Pesticides in Foods and Agricultural Samples


    This month's instalment of "Sample Prep Perspectives" describes a new extraction technique called QuEChERS (standing for quick, easy, cheap, effective and safe and is pronounced "catchers") for the sample preparation of pesticides in foods and agricultural samples. The technique uses simple glassware, a minimal amount of organic solvent and various salt/buffer additives to partition analytes into an organic phase for clean up by dispersive solid-phase extraction (d-SPE). The technique provides good recoveries, is reproducible and costs less than other sample preparation approaches. The technique is being adopted by many laboratories worldwide. It has the potential for applications outside of the pesticide in foods area.

    The Determination of Furan in Foods — Challenges and Solutions


    The determination of the carcinogenic food processing contaminant furan by headspace sampling of foods is challenging because it can easily escape from the sample during preparation. Furan can also be easily formed as a by-product when the sample is heated in the headspace apparatus. This article describes a number of approaches to overcome these difficulties and alternative methods to quantify furan in a variety of matrices.

    Advanced Topics in Solid-Phase Extraction: Chemistries


    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.

    Modern Techniques for the Extraction of Solid Materials — An Update


    Traditional methods for the sample preparation of insoluble solid materials have represented one of the more time consuming and labour-intensive efforts in analysis. In this instalment of "Sample Prep Perspectives", Ron Majors examines modern sample preparation methods for solids that often involve increased temperature and higher pressure to speed up the extraction process. In addition, modern sample preparation methods have been automated to relieve analysts of the drudgery associated with traditional methods. Here, he reports on automated Soxhlet extraction, supercritical fluid extraction, pressurized fluid extraction–accelerated solvent extraction, and microwave-assisted extraction and updates earlier coverage.

    The Possibilities and Limitations of Capillary Extraction (CEx): The Case Study of Polycyclic Aromatic Hydrocarbons (PAHs) in Clean-water Samples


    Capillary extraction (CEx) is used to study the solventless in-tube extraction of naphthalene, acenaphthene, phenanthrene, fluoranthene, chrysene, benzo(a)pyrene and coronene in aqueous samples prepared by analyte spiking into clean waters or, as an alternative, by using the generator–column method of sample preparation. Analysis of laden extractors is conveniently performed by high-resolution gas chromatography (GC), with a flameionization detector (FID). Extraction set-ups and main extraction variables are investigated from a practical point of view. For 2- to 4-ring polycyclic aromatic hydrocarbons (PAHs), equilibrium times are within a few minutes, analytical sensitivity is in the parts-per-billion (ppb) range and reproducibility is better than 10% relative standard deviation (RSD) (n = 6). Coronene behaviour is unique and presumably determined by extreme hydrophobicity and thus very negligible aqueous solubility: in-tube extraction of coronene seems possible only if starting from oversaturated..

    The Role of Passive Samplers in the Monitoring of Aquatic Ecosystems and Occupational Hygiene Pollution


    Commercialization of the passive sampler is very important because it reflects acceptance by the wider community.

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