Sample pretreatment is the most important procedure to remove the matrix for interfacing with mass spectrometry (MS). Additionally, for the samples with low concentration, the process of preconcentration is required before MS analysis. We have newly developed a solid-phase extraction stationary phase based on C60-fullerene covalently bound to silica for purification of biomolecules of different characteristics. Silica particles of different porosity are modified with aminopropyl linker and then covalently bound to C60-fullerenoacetic acid or C60-epoxyfullerenes. The developed materials have been successfully applied as an alternative to commercially available reversed-phase materials for solid-phase extraction. C60-fullerene silica is able to retain small and hydrophilic molecules like phosphopeptides, which can be easily lost by reversed-phase sorbents. The novel materials are applied for desalting and preconcentration of proteins and peptides, especially phosphopeptides. In addition, the C60-fullerene silica is applied for the solid-phase extraction of selected flavonoids with recoveries of approximately 99%. The recoveries are compared with the commercially available solid-phase extraction materials.
This review covers recent applications of near infrared (NIR) spectroscopy in the determination of physico-chemical and morphological parameters of polymeric materials. Near infrared measurements in the diffuse reflection mode are highlighted, which analyse the structural parameters such as porosity, surface area and particle size. Fundamentals and applications of the technique are discussed and examples of quantitative and qualitative analysis are explained. Various approaches like on-and in-line techniques, bulk measurements and kinetic studies for recording spectra are discussed. Furthermore, this review addresses the development of calibrations, which allow for the differentiation and quantification of materials with varying physical and morphological properties. Parameters like constitution, composition and crystallinity have a strong affect on the material characteristics. Therefore, chemical, physical and mechanical properties of synthetic as well as natural substances, such as polymeric composites and cotton or wool, need to be studied in-depth. To sum up, NIR spectroscopy has been developed as a flexible, robust and high-throughput analytical method that can be combined with chemometric and multivariate data analysis for fast and reliable screening in material science.
Fourier-transform infrared (FT-IR) based mapping and imaging is a fast emerging technology which is being increasingly applied to investigate tissues in the high-throughput mode. The high resolution close to the cellular level, the possibility to determine the bio-distribution of molecules of interest (proteins, peptides, lipids, carbohydrates) without any pre-treatment and the offer to yield molecular structure information have brought evidence that this technique allows to gain new insights in cancer pathology. Thus, several individual mainly protein and peptide cancer markers ("biomarkers") can be identified from FT-IR tissue images, enabling accurate discrimination between healthy and tumour areas. Optimal data acquisition (spatial resolution, spectral resolution, signal to noise ratio), classification, and validation are necessary to establish practical protocols that can be translated to the qualitative and quantitative clinical routine analysis. Thereby, the development of modern fast infrared imaging systems has strongly supported its acceptance in clinical histopathology. In this review, the necessity of analysis based on global cancer statistics, instrumental setups and developments, experimental state of the art are summarised and applications to investigate different kinds of cancer (e.g., prostate, breast, cervical, colon, oral cavity) are shown and discussed in detail.
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